CN106589903A - Preparation method and application of graphene polyurethane nanocomposite - Google Patents
Preparation method and application of graphene polyurethane nanocomposite Download PDFInfo
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- CN106589903A CN106589903A CN201611129047.3A CN201611129047A CN106589903A CN 106589903 A CN106589903 A CN 106589903A CN 201611129047 A CN201611129047 A CN 201611129047A CN 106589903 A CN106589903 A CN 106589903A
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- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
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- C—CHEMISTRY; METALLURGY
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- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
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- C08L2201/00—Properties
- C08L2201/14—Gas barrier composition
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Abstract
The invention discloses a preparation method and an application of a graphene polyurethane nanocomposite. A mixture of graphite, a polyurethane emulsion or solution and a small quantity of processing aids are subjected to shear grinding, so that graphite is directly stripped off graphene sheets and is composited in situ with a polymer; then remaining graphite is separated by high-speed centrifugation, and graphene polyurethane composite slurry is obtained. The graphene polyurethane nanocomposite can be used in fields such as gas barrier packaging materials, anti-corrosion coating materials, conductive film, conductive resin and the like. The preparation method of the nanocomposite has the advantages that the technological process is greatly simplified, during stripping, polymer segments are intercalated into the graphite sheets, stripping of graphene is facilitated, the polymer segments can play a role in hindering the graphene sheets from being aggregated again after the composite slurry is formed, and accordingly, the stability of a dispersion system is guaranteed.
Description
Technical field
The present invention relates to the preparation method and purposes of Graphene polyurethane nano composite material, belong to polymer composite
Field.
Background technology
In recent years Graphene polymer composite is with its excellent electric conductivity, barrier property, and electromagnetic wave shielding
Can, by the extensive concern of relevant industries.Effective Graphene network wherein how is formed, and reduces preparing overall cost,
To realize the extensive application of material, become research emphasis.At present the preparation method of Graphene polyurethane nano composite material is all
With Graphene as raw material, disperseed with polymer mixed by complicated complex method.On the one hand Graphene in the market
On the high side, on the other hand complicated complex method not only may not be certain to improve the stroke of Graphene network, greatly improve on the contrary
The cost of material, limits its application.With graphite as raw material, one-step method prepares the method for Graphene polyurethane not only it
Feasibility, also possesses very big advantage.
The content of the invention
The purpose of the present invention is for the deficiencies in the prior art, there is provided one kind completes Graphene by raw material one-step method of graphite
With the preparation of graphene nanocomposite material, the purpose of the present invention is by following technical measures realization：
Graphene polyurethane nano composite material is, by graphite, polyaminoester emulsion or solution and a small amount of processing aid, to lead to
Crossing the method for shearing grinding makes graphite directly separate graphene sheet layer, compound with polymer in situ, then by high speed centrifugation point
Remaining graphite is separated out, Graphene polyurethane composite mortar is obtained.Further construction is needed to form conductive composite wood according to application
Material.Described graphite, polyaminoester emulsion or solution and processing aid, according to parts by weight be followed successively by 2～11 parts, 78～97
Part, 0.3～3 part.
Used graphite is existing crystalline flake graphite, expansible graphite and expanded graphite on market.
The medium of grinding is all kinds polyaminoester emulsion or polyurethane solutions that solid content is 15～65%.
In preparation process, can be according to abrasive media viscosity, and medium is helped with a small amount of processing of interaction force addition of graphite
Agent, such as thickening agent, thinner, surfactant etc..
Equipment for grinding can be planetary ball mill, conical ball mill, horizontal ball mill, high-speed shearing emulsion machine etc.
Equipment with shearing grinding function.
Specific preparation process is comprised the following steps：
1), graphite is added and is uniformly mixed in polyaminoester emulsion or solution, and be slowly stirred it is lower place 30～
80min, makes polymer segment be intercalation in advance as far as possible in graphite flake layer, adds a small amount of processing aid to adjust viscosity.
2), the mixture in 1) is placed in shearing milling apparatus, appropriate rotating speed and milling time is adjusted, is shelled from graphite
Separate out Graphene.And remaining graphite is gone out by high speed centrifugation sub-argument, obtain Graphene polyurethane composite mortar.
3) select rational construction method to be processed further in the slurry for obtaining, that is, obtain Graphene polyurethane nano and be combined
Material.
In process of lapping, different according to the selection of milling apparatus, milling time is usually 1.5～6h, and equipment rotating speed is usual
For 150～600 turns, for high speed shearing emulsification agent, rotating speed need to be adjusted suitably.
The Graphene polyurethane composite mortar can be used to prepare the good bag of barrier properties for gases by different construction methods
The fields such as package material, or erosion shield material, conductive film, electroconductive resin.
During application and construction, according to the performance requirement of target product, related auxiliaries can be coordinated, and will not be to material
The performance of itself is adversely affected.The auxiliary agent that can be used cooperatively also includes that defoamer, levelling agent, coupling agent, rheological agent, light are steady
Determine agent, antioxidant, biocide mildewcide etc..
The preparation method and purposes of the Graphene polyurethane nano composite material that the present invention is provided, its technique side prepares nanometer
Composite technology flow process is greatly simplified, and in stripping process, polymer segment intercalation is entered between graphite flake layer, is conducive to Graphene
Stripping, after forming composite mortar, polymer segment can play a part of to hinder graphene sheet layer to reunite again, to guarantee point
The stability of prose style free from parallelism system.
Specific embodiment
The present invention is specifically described below by embodiment, it is necessary to which again this is pointed out that the present embodiment is served only for
To further illustrating that the present invention is carried out, it is impossible to be interpreted as limiting the scope of the invention, person skilled in art can
To make some nonessential modifications and adaptations according to the content of foregoing invention.
Embodiment 1
The expanded graphite of 4g is added in the DMF solution of 95g polyurethane and is uniformly mixed, and put under slow stirring
30min is put, polymer segment is intercalation in advance as far as possible in graphite flake layer, the auxiliary agent for adding 0.75% adjusts viscosity.Will mixing
Thing is placed in planetary ball mill instrument, and it is 3h to adjust rotating speed 200r/min and milling time.Finally by the residue that is centrifuged at a high speed out
Graphite, obtain Graphene polyurethane composite mortar.The slurry for obtaining is coated on into metal device surface, is dried in 80 DEG C of baking ovens
One layer of corrosion inhibiting gas barrier coat for being evenly distributed on polymer surfaces is obtained, it is to avoid device during storage and transport
Environmental corrosion.
Embodiment 2
The expanded graphite of 6g is added in the DMF solution of 93g polyurethane and is uniformly mixed, and put under slow stirring
30min is put, polymer segment is intercalation in advance as far as possible in graphite flake layer, the auxiliary agent for adding 0.33% adjusts viscosity.Will mixing
Thing is placed in high-speed shearing emulsion machine, and it is 3.5h to adjust rotating speed 200r/min and milling time.Finally by being centrifuged at a high speed
Go out remaining graphite, obtain Graphene polyurethane composite mortar.Rational construction method is selected further to add in the slurry for obtaining
Work, that is, obtain Graphene polyurethane nano composite material.
Embodiment 3
The expanded graphite of 3.5g is added in the DMF solution of 92g polyurethane and is uniformly mixed, and under slow stirring
40min is placed, polymer segment is intercalation in advance as far as possible in graphite flake layer, the auxiliary agent for adding 0.45% adjusts viscosity.Will be mixed
Compound is placed in planetary ball mill instrument, and it is 2h to adjust rotating speed 300r/min and milling time.It is surplus finally by being centrifuged at a high speed out
Remaining graphite, obtains Graphene polyurethane composite mortar.Rational construction method is selected to be processed further in the slurry for obtaining, i.e.,
Obtain Graphene polyurethane nano composite material.
Embodiment 4
The crystalline flake graphite of 9g is added in the DMF solution of 87g polyurethane and is uniformly mixed, and put under slow stirring
30min is put, polymer segment is intercalation in advance as far as possible in graphite flake layer, the auxiliary agent for adding 0.3% adjusts viscosity.By mixture
In being placed in planetary ball mill instrument, it is 2.5h to adjust rotating speed 200r/min and milling time.Finally by the residue that is centrifuged at a high speed out
Graphite, obtain Graphene polyurethane composite mortar.Select rational construction method to be processed further in the slurry for obtaining, obtain final product
To Graphene polyurethane nano composite material.
Embodiment 5
The crystalline flake graphite of 6.2g is added in the DMF solution of 82g polyurethane and is uniformly mixed, and under slow stirring
30min is placed, polymer segment is intercalation in advance as far as possible in graphite flake layer, the auxiliary agent for adding 0.5% adjusts viscosity.Will mixing
Thing is placed in planetary ball mill instrument, and it is 3h to adjust rotating speed 200r/min and milling time.Finally by the residue that is centrifuged at a high speed out
Graphite, obtain Graphene polyurethane composite mortar.Select rational construction method to be processed further in the slurry for obtaining, obtain final product
To Graphene polyurethane nano composite material.
Embodiment 6
The crystalline flake graphite of 4g is added in the DMF solution of 91g polyurethane and is uniformly mixed, and put under slow stirring
30min is put, polymer segment is intercalation in advance as far as possible in graphite flake layer, the auxiliary agent for adding 0.25% adjusts viscosity.Will mixing
Thing is placed in planetary ball mill instrument, and it is 3.5h to adjust rotating speed 250r/min and milling time.It is surplus finally by being centrifuged at a high speed out
Remaining graphite, obtains Graphene polyurethane composite mortar.Rational construction method is selected to be processed further in the slurry for obtaining, i.e.,
Obtain Graphene polyurethane nano composite material.
Embodiment 7
The expanded graphite of 6g is added in the aqueous polyurethane emulsion of 92g solid contents 35% and is uniformly mixed, and
Lower placement 10min is slowly stirred, the auxiliary agent for adding 0.15% adjusts viscosity.Mixture is placed in conical ball mill, is adjusted and is turned
Fast 350r/min and milling time are 2.5h.Finally by the remaining graphite that is centrifuged at a high speed out, Graphene polyurethane is obtained
Composite mortar.Select rational construction method to be processed further in the slurry for obtaining, that is, obtain Graphene polyurethane nano and be combined
Material.
Embodiment 8
The expansible graphite of 4.5g is added to into 82g, is uniformly mixed in 35% aqueous polyurethane emulsion, and slow
Slow stirring is lower to place 15min, and the auxiliary agent for adding 3.5% adjusts viscosity.Mixture is placed in horizontal ball mill, rotating speed is adjusted
550r/min and milling time are 4.5h.Finally by the remaining graphite that is centrifuged at a high speed out, obtain Graphene polyurethane and answer
Close slurry.Select rational construction method to be processed further in the slurry for obtaining, that is, obtain Graphene polyurethane nano composite wood
Material.
Embodiment 9
The expanded graphite of 11g is added to into 78g, solid content be 15% aqueous polyurethane emulsion in mix homogeneously, and
Lower placement 20min is slowly stirred, polymer segment is intercalation in advance as far as possible in graphite flake layer, the auxiliary agent for adding 2.5% is adjusted
Viscosity.Mixture is placed in horizontal ball mill, it is 6h to adjust rotating speed 150r/min and milling time.Finally by high speed centrifugation
Remaining graphite is isolated, Graphene polyurethane composite mortar is obtained.Rational construction method is selected to enter one in the slurry for obtaining
Step processing, that is, obtain Graphene polyurethane nano composite material.
Embodiment 10
The expansible graphite of 9g is added to into 85g, solid content be 65% aqueous polyurethane emulsion in mix homogeneously, and
Decentralization is slowly stirred, 25min, the auxiliary agent for adding 5.5% adjusts viscosity.Mixture is placed in planetary ball mill instrument, rotating speed is adjusted
200r/min and milling time are 5h.Finally by the remaining graphite that is centrifuged at a high speed out, obtain Graphene polyurethane and be combined
Slurry.Select rational construction method to be processed further in the slurry for obtaining, that is, obtain Graphene polyurethane nano composite material.
Embodiment 11
The expanded graphite of 7g is added in the DMF solution of 82g polyurethane and is uniformly mixed, and put under slow stirring
30min is put, polymer segment is intercalation in advance as far as possible in graphite flake layer, the auxiliary agent for adding 4.5% adjusts viscosity.By mixture
In being placed in high-speed shearing emulsion machine, it is 1.5h to adjust rotating speed 3000r/min and milling time.Finally by being centrifuged at a high speed out
Remaining graphite, obtains Graphene polyurethane composite mortar.Rational construction method is selected to be processed further in the slurry for obtaining,
Obtain Graphene polyurethane nano composite material.
Embodiment 12
The expanded graphite of 11g is added in the DMF solution of 83g polyurethane and is uniformly mixed, and under slow stirring
40min is placed, polymer segment is intercalation in advance as far as possible in graphite flake layer, the auxiliary agent for adding 2.5% adjusts viscosity.Will mixing
Thing is placed in planetary ball mill instrument, and it is 3h to adjust rotating speed 300r/min and milling time.Finally by the residue that is centrifuged at a high speed out
Graphite, obtain Graphene polyurethane composite mortar.Select rational construction method to be processed further in the slurry for obtaining, obtain final product
To Graphene polyurethane nano composite material.
Claims (8)
1. Graphene polyurethane nano composite material, it is characterised in that be prepared by the following method gained, graphite, polyurethane breast
Liquid or solution and processing aid, make graphite directly separate graphene sheet layer by the method for shearing grinding, former with polymer
Position is compound, then by the remaining graphite that is centrifuged at a high speed out, obtains Graphene polyurethane composite mortar.
2. Graphene polyurethane nano composite material according to claim 1, it is characterised in that comprise the following steps：
1), graphite is added and is uniformly mixed in polyaminoester emulsion or solution, and be slowly stirred 30～80min of lower placement, made
Polymer segment is intercalation in advance as far as possible in graphite flake layer, adds processing aid to adjust viscosity；
2), the mixture in 1) is placed in shearing milling apparatus, appropriate rotating speed and milling time is adjusted, is separated from graphite
Graphene；And remaining graphite is gone out by high speed centrifugation sub-argument, obtain Graphene polyurethane composite mortar.
3), select rational construction method to be processed further in the slurry for obtaining, that is, obtain Graphene polyurethane nano composite wood
Material.
3. Graphene polyurethane nano composite material according to claim 2, it is characterised in that described graphite, polyurethane
Emulsion or solution and processing aid, according to parts by weight 2～11 parts, 78～97 parts, 0.3～3 part are followed successively by.
4. Graphene polyurethane nano composite material according to claim 3, it is characterised in that described graphite is scale stone
One kind in ink, expansible graphite and expanded graphite.
5. Graphene polyurethane nano composite material according to claim 3, it is characterised in that described polyaminoester emulsion or
The solid content of solution is 15～65%.
6. Graphene polyurethane nano composite material according to claim 3, it is characterised in that described processing aid is to increase
Thick dose, thinner, surfactant.
7. Graphene polyurethane nano composite material according to claim 2, it is characterised in that step 3) construction method
In, according to the performance requirement of target product, the related adjuvant of addition, and negative shadow will not be caused to the performance of material itself
Ring, adjuvant includes defoamer, levelling agent, coupling agent, rheological agent, light stabilizer, antioxidant, biocide mildewcide.
8. according to any one of claim 1 to 7 Graphene polyurethane nano composite material purposes, it is characterised in that use
In preparing the good packaging material of barrier properties for gases, or erosion shield material, conductive film, electroconductive resin.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611129047.3A CN106589903A (en) | 2016-12-09 | 2016-12-09 | Preparation method and application of graphene polyurethane nanocomposite |
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| CN201611129047.3A CN106589903A (en) | 2016-12-09 | 2016-12-09 | Preparation method and application of graphene polyurethane nanocomposite |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019095642A1 (en) * | 2017-11-20 | 2019-05-23 | 曹熙辰 | Anti-corrosion coating composition, method for preparing anti-corrosion coating, and anti-corrosion coating |
| CN110741033A (en) * | 2017-05-05 | 2020-01-31 | 迪热克塔普拉斯股份公司 | Polyurethane film comprising graphene and method for preparing same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101864005A (en) * | 2010-06-03 | 2010-10-20 | 华侨大学 | Method for preparing polymer/graphene composite material |
| CN105712334A (en) * | 2014-12-01 | 2016-06-29 | 江阴碳谷科技有限公司 | Viscous graphene stripping combined solution |
| CN105869770A (en) * | 2016-03-30 | 2016-08-17 | 成都新柯力化工科技有限公司 | Graphene conductive paste prepared by mechanical stripping and preparation method of graphene conductive paste |
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2016
- 2016-12-09 CN CN201611129047.3A patent/CN106589903A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101864005A (en) * | 2010-06-03 | 2010-10-20 | 华侨大学 | Method for preparing polymer/graphene composite material |
| CN105712334A (en) * | 2014-12-01 | 2016-06-29 | 江阴碳谷科技有限公司 | Viscous graphene stripping combined solution |
| CN105869770A (en) * | 2016-03-30 | 2016-08-17 | 成都新柯力化工科技有限公司 | Graphene conductive paste prepared by mechanical stripping and preparation method of graphene conductive paste |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110741033A (en) * | 2017-05-05 | 2020-01-31 | 迪热克塔普拉斯股份公司 | Polyurethane film comprising graphene and method for preparing same |
| US11512175B2 (en) | 2017-05-05 | 2022-11-29 | Directa Textile Solutions S.R.L. | Polyurethane film comprising graphene and preparation process thereof |
| WO2019095642A1 (en) * | 2017-11-20 | 2019-05-23 | 曹熙辰 | Anti-corrosion coating composition, method for preparing anti-corrosion coating, and anti-corrosion coating |
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Application publication date: 20170426 |