CN103980750A - Graphene spray as well as preparation method and application thereof - Google Patents
Graphene spray as well as preparation method and application thereof Download PDFInfo
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- CN103980750A CN103980750A CN201410241009.1A CN201410241009A CN103980750A CN 103980750 A CN103980750 A CN 103980750A CN 201410241009 A CN201410241009 A CN 201410241009A CN 103980750 A CN103980750 A CN 103980750A
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Abstract
The invention discloses a graphene spray as well as a preparation method and application thereof. The graphene spray comprises a graphene solution and a photocatalyst mixing solution. The graphene catalyst can form a waterproof breathable graphene film with excellent performances on the surface of outdoor supplies, and is low in price, simple to prepare, convenient to carry, and simple to use.
Description
Technical field
The present invention relates to a kind of spray of being made by Graphene, concrete preparation method and the purposes of this spray.
Background technology
In recent years, along with mountain-climbing, skiing, the outdoor activity such as navigation flourish, to footwear, clothes, cap, tent, sleeping bag, the waterproof and breathable functional requirement of these outdoor goods of moisture barrier bag is very strong.These outdoor goods integrate waterproof, moisture-inhibiting, windproof, warming, and it can resist the invasion of sleet and cold wind, can allow again the sweat gas of human body discharge in time, keeps dry and comfortable and warm, thereby realizes the unification of articles for use water-proof function and comfortableness.And traditional material is airtight, while dress, feel stuffy, the sweat that human body produces cannot be discharged to outside, builds up condensation at internal surface, makes people feel uncomfortable and has clammy sense, even has frostbite, and the situation of freezing to death occurs.
Along with scientific and technical development, the mode that starts to adopt coating or film to form one deck waterproof ventilated membrane on these outdoor goods surfaces solves foregoing problems.Waterproof ventilated membrane has experienced following four generations at present:
The first-generation: the earliest in order to reach waterproof, windproof, just cover waterproof glue on fabric, to reach waterproof object, the product that this material and technique are made, can resistance to certain hydraulic pressure, but can never breathe freely, and water-proof breathable properties is poor.
The s-generation: PU film, this is all well and good material of a kind of water pressure resistance, and product fabric is combined with each other with it, can accomplish that anti-water stability is better, its high-end product also has a little moisture-inhibiting function, but effect is very undesirable.As: the existing KING-TEX in market.
The third generation: TPU film, on PU Membranous Foundations, develop, all making moderate progress aspect ventilative, moisture-inhibiting, water pressure resistance than PU film, be a kind of waterproof ventilated membrane that substitutes PU film, domestic have TING-TEX, a KING-TEX etc.
The 4th generation: EPTFE film (tetrafluoroethylene) is latest generation waterproof ventilated membrane, and its water-proof breathable properties is all better.There are mainly containing of outstanding performance: GORE-TEX (development of W. L. Gore & Associates, Inc. company), OMNI-TECH (development of COLUMBIA company of the U.S.), FIRST-TEX (development of FBA global group of the U.S.), EVENT (the waterproof and breathable specialized material business development emerging rapidly in recent years), TEXPORE (German JACKWOLFSKIN company development) etc. in world market.But this film price is more expensive, easy to wear after long-time use, and repair difficult expensive.
Sum up thus existing waterproof ventilated membrane and have following three defects: (1) existing common waterproof ventilated membrane, water-repellancy and ventilation property are poor.(2) existing good waterproof ventilated membrane, waterproof and ventilation property are better still expensive.(3) easy to wear after existing waterproof ventilated membrane life-time service, and repair difficulty, expensive.
Summary of the invention
The object of the invention is to solve the various defects of aforesaid waterproof ventilated membrane, provide one to prepare simply, easy to carry, use articles for use surface simply out of doors form Graphene spray of the graphene film of the well behaved water-proof breathable properties of one deck and preparation method thereof using and as the application of waterproof ventilated membrane.
First the technical scheme that realizes the object of the invention is a kind of Graphene spray, is made up of graphene solution and photocatalyst mixing solutions; The concentration of the photocatalyst adding in described graphene solution is 0.01～1mg/ml; Described photocatalyst is titanium dioxide or zinc oxide or stannic oxide or zirconium dioxide or Cadmium Sulfide.
Next is the preparation method of this Graphene spray, comprises the following steps:
Step 1: prepare Graphene powder: adopt oxidation reduction process to prepare Graphene powder; In ice-water bath, prepare the reaction flask of 250ml～1000ml; Then the vitriol oil that adds 200～600ml concentration to be greater than 70%, adds the solid mixt of 2～8g Graphite Powder 99 and 1～4g SODIUMNITRATE under stirring, stirring velocity is 100rpm～300rpm, churning time 10～20min; Then divide six times and add 6～24g potassium permanganate, stirring velocity is 100rpm～300rpm, and churning time 10～20min is warming up to 25 DEG C～35 DEG C subsequently, and continues to stir, and stirring velocity is 300rpm～500rpm, stirs 20min～30min; Slowly add 100～300ml deionized water, continue to stir 20～30min; Be warming up to 90 DEG C～100 DEG C and keep 20min～1h, adding 10～30ml massfraction is that 40%～65% aqueous hydrogen peroxide solution reduces residual oxygenant, and is uniformly mixed, and then leaves standstill 0.5h～1h; Employing is greater than the ultrapure water of 18M Ω * cm and 5～10% salt acid elution by resistivity, until sulfate radical-free is detected in filtrate; Finally solution is filtered, screening is placed in to the fully dry Graphene powder that obtains of 50～60 DEG C of vacuum drying ovens.
Step 2: prepare graphene solution: add solvent in the graphene powder preparing, after mixing and mixing, mixed solution is placed on ultrasonator and is shaken, ultrasonic power is 200W, ultrasonic frequency is 60KHZ, ultrasonic concussion time 1～3h, obtains the graphene solution that concentration is 0.5～15mg/ml.Solvent is the mixture of water or organic solvent or at least two kinds of organic solvents; Described organic solvent is methyl alcohol or ethanol or Virahol or acetone or ethyl acetate or chloroform or tetracol phenixin or tetrahydrofuran (THF) or DMF or dimethyl sulfoxide (DMSO) or benzene or toluene or dimethylbenzene or chlorobenzene or dichlorobenzene or trichlorobenzene; Preferred solvent is one or any two or more the mixture of organic solvent in water, methyl alcohol, ethanol, acetone, ethyl acetate, chloroform, tetrahydrofuran (THF), benzene, toluene.More preferably one or any two or more the mixture of organic solvent in water, ethanol, acetone, ethyl acetate, chloroform; Most preferred solvent is water or ethanol.
Step 3: prepare spray solution: to the photocatalyst that adds 0.01～1mg/ml in the graphene solution in step 2, first adopt ultrasonic oscillation fully loose to mixing solutions; Described ultrasonic power is 200W, and ultrasonic frequency is 60KHZ, and the ultrasonic oscillation time is 1～3h; Subsequently mixing solutions is carried out to centrifugal purification processing, described centrifugal rotational speed is 4000rpm～12000rpm, and centrifugation time is 1～30min; Preferably centrifugation time is 10～20min.Get the supernatant liquor of centrifugal rear Graphene and photocatalyst as spraying agent.Photocatalyst is titanium dioxide or zinc oxide or stannic oxide or zirconium dioxide or Cadmium Sulfide; Be preferably titanium dioxide.
Finally, the present invention also comprises the application to aforementioned Graphene spray, with Graphene spray, outdoor goods surface is carried out the application of waterproof and breathable processing, by direct articles for use out of doors surface after outdoor goods surface spraying being formed to the graphene film of waterproof and breathable.The thickness of the graphene film that after described spraying, articles for use surface forms is out of doors 0.1～100 μ m; Be preferably 1～80 μ m, more preferably 5～60 μ m, most preferably are 10～50 μ m.The described method that the processing of graphite spraying alkene spray is carried out in outdoor goods surface is: the required spraying outdoor goods of nozzle distance surface is 1～15cm, is preferably 2～12cm, and more preferably 2～10cm, most preferably is 5～8cm; The time range of spraying is 0.5～10min, is preferably 1～8min, and more preferably 1～5min, most preferably is 2～4min; Spraying, for spraying at any angle, is preferably continuous spray at any angle, more preferably the continuous spray at any angle of circulation; After spraying, outdoor goods is dried naturally to flash-off time 10～30min.
The present invention is based on the research to Graphene, if confirm to adopt Graphene can make full use of the following performance of Graphene as waterproof ventilated membrane: (1) Graphene is the highest material of mankind's known strength, also harder than diamond, strength ratio taller upper 100 times of best iron and steel in the world, therefore adopts Graphene can have good surface strength and wear resisting property as waterproof ventilated membrane; (2) Graphene price lattice are cheap; (3) single-layer graphene thickness is 0.34nm, and it is almost completely transparent, and having the good infiltrative while for outdoor goods surface can not affect the appearance luster of outdoor goods; (4) Graphene itself has hydrophobicity, and the diameter of water droplet is at 4～50mm, and the size of stream molecule is about 0.4nm, so Graphene can allow water molecules pass through in stopping water droplet, has good water-repellancy and ventilation property.(5) Graphene can bacteria growing inhibiting, can reduce the injury of bacterium to human body in the situation of field for outdoor goods.
Thus, the present invention has following useful effect: (1) the present invention proposes a kind of Graphene waterproof and breathable spray, articles for use surfaces forms the graphene film of the water-proof breathable properties of one deck premium properties out of doors, low price, prepare simple, easy to carry, use simple.
(2) Graphene spray of the present invention has added photocatalyst, can be formed directly in graphene film after spraying.Instead of graphene oxide is again through going back original production graphene film, does not need heating or baking, therefore easy to use, user can arrange the waterproof and breathable protective membrane of superior performance whenever and wherever possible for the outdoor goods of oneself.
(3) Graphene spray of the present invention adopts titanium dioxide as photocatalyst, can further have that catalytic performance is good, stable chemical performance, safety non-toxic, have no side effect, the advantage such as cheap, long service life.
(4) nano level Graphene spray of the present invention has good perviousness on articles for use surface, forms stable protective membrane.
(5) Graphene spray of the present invention can form and have good surface strength, wear resistance, ventilation property, water-repellancy, bactericidal protective membrane.
(6) after the water-proof breathable properties of graphene film of the present invention lost efficacy, can again spray spray and again form protective membrane, very convenient.
Embodiment
The preparation method of Graphene spray, comprises the following steps:
Step 1: prepare Graphene powder: adopt oxidation reduction process to prepare Graphene powder; In ice-water bath, prepare the reaction flask of 250ml～1000ml; Then the vitriol oil that adds 200～600ml concentration to be greater than 70%, adds the solid mixt of 2～8g Graphite Powder 99 and 1～4g SODIUMNITRATE under stirring, stirring velocity is 100rpm～300rpm, churning time 10～20min; Then divide six times and add 6～24g potassium permanganate, stirring velocity is 100rpm～300rpm, and churning time 10～20min is warming up to 25 DEG C～35 DEG C subsequently, and continues to stir, and stirring velocity is 300rpm～500rpm, stirs 20min～30min; Slowly add 100～300ml deionized water, continue to stir 20～30min; Be warming up to 90 DEG C～100 DEG C and keep 20min～1h, adding 10～30ml massfraction is that 40%～65% aqueous hydrogen peroxide solution reduces residual oxygenant, and is uniformly mixed, and then leaves standstill 0.5h～1h; Employing is greater than the ultrapure water of 18M Ω * cm and 5～10% salt acid elution by resistivity, until sulfate radical-free is detected in filtrate; Finally solution is filtered, screening is placed in to the fully dry Graphene powder that obtains of 50～60 DEG C of vacuum drying ovens.
Step 2: prepare graphene solution: add solvent in the graphene powder preparing, after mixing and mixing, mixed solution is placed on ultrasonator and is shaken, ultrasonic power is 200W, ultrasonic frequency is 60KHZ, ultrasonic concussion time 1～3h, obtains the graphene solution that concentration is 0.5～15mg/ml.Solvent is the mixture of water or organic solvent or at least two kinds of organic solvents; Described organic solvent is methyl alcohol or ethanol or Virahol or acetone or ethyl acetate or chloroform or tetracol phenixin or tetrahydrofuran (THF) or DMF or dimethyl sulfoxide (DMSO) or benzene or toluene or dimethylbenzene or chlorobenzene or dichlorobenzene or trichlorobenzene; Preferred solvent is one or any two or more the mixture of organic solvent in water, methyl alcohol, ethanol, acetone, ethyl acetate, chloroform, tetrahydrofuran (THF), benzene, toluene.More preferably one or any two or more the mixture of organic solvent in water, ethanol, acetone, ethyl acetate, chloroform; Most preferred solvent is water or ethanol.Organic solvent contributes in dissolving dispersed graphite alkene powder, and in the solution of preparation, Graphene is uniformly dispersed.
Step 3: prepare spray solution: to the photocatalyst that adds 0.01～1mg/ml in the graphene solution in step 2, first adopt ultrasonic oscillation fully loose to mixing solutions; Described ultrasonic power is 200W, and ultrasonic frequency is 60KHZ, and the ultrasonic oscillation time is 1～3h; Subsequently mixing solutions is carried out to centrifugal purification processing, described centrifugal rotational speed is 4000rpm～12000rpm, and centrifugation time is 1～30min; Preferably centrifugation time is 10～20min, can guarantee that solution homogeneity is better.Get the supernatant liquor of centrifugal rear Graphene and photocatalyst as spraying agent.Photocatalyst is titanium dioxide or zinc oxide or stannic oxide or zirconium dioxide or Cadmium Sulfide; Be preferably titanium dioxide.
Make after Graphene spray, by direct articles for use out of doors surface after outdoor goods surface spraying being formed to the graphene film of waterproof and breathable.The thickness of the graphene film that after spraying, articles for use surface forms is out of doors 0.1～100 μ m; Be preferably 1～80 μ m, more preferably 5～60 μ m, most preferably are 10～50 μ m.The method of outdoor goods surface being carried out to the processing of graphite spraying alkene spray is: the required spraying outdoor goods of nozzle distance surface is 1～15cm, is preferably 2～12cm, and more preferably 2～10cm, most preferably is 5～8cm; The time range of spraying is 0.5～10min, is preferably 1～8min, and more preferably 1～5min, most preferably is 2～4min; Spraying, for spraying at any angle, is preferably continuous spray at any angle, more preferably the continuous spray at any angle of circulation; After spraying, outdoor goods is dried naturally to flash-off time 10～30min.The waterproof ventilated membrane that graphene film forms can again spray spray and again form protective membrane after losing efficacy.
Carry out nine groups of application below and be listed as and detect, table one is the selection of nine application row, the result that the graphene film that table two forms for the spray that nine application row are made detects.
Table one: nine application examples
Table two: nine application examples detected results
From the detected result of table two, the outdoor goods waterproof ventilated membrane with high-performance that Graphene spray of the present invention can be used as latest generation completely uses.
Above-described specific embodiment; object of the present invention, technical scheme and beneficial effect are further described; institute is understood that; the foregoing is only specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any amendment of making, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (10)
1. a Graphene spray, is characterized in that: be made up of graphene solution and photocatalyst mixing solutions.
2. Graphene spray according to claim 1, is characterized in that: the concentration of described photocatalyst in mixing solutions is 0.01～1mg/ml.
3. a kind of Graphene spray according to claim 2, is characterized in that: described photocatalyst is titanium dioxide or zinc oxide or stannic oxide or zirconium dioxide or Cadmium Sulfide, preferably titanium dioxide.
4. a preparation method for Graphene spray, is characterized in that comprising the following steps:
Step 1: prepare Graphene powder: adopt oxidation reduction process to prepare Graphene powder;
Step 2: prepare graphene solution: add solvent in the graphene powder preparing, obtain graphene solution after stirring and evenly mixing;
Step 3: prepare spray solution: add photocatalyst in the graphene solution in step 2, mixing solutions is carried out to centrifugal purification processing, get the supernatant liquor of centrifugal rear Graphene and photocatalyst as spraying agent.
5. the preparation method of a kind of Graphene spray according to claim 4, is characterized in that: the photocatalyst that adds 0.01～1mg/ml in described step 3; Described photocatalyst is titanium dioxide or zinc oxide or stannic oxide or zirconium dioxide or Cadmium Sulfide; Be preferably titanium dioxide.
6. the preparation method of a kind of Graphene spray according to claim 5, is characterized in that: after adding photocatalyst, first adopt ultrasonic oscillation that it is fully disperseed to mixing solutions; Described ultrasonic power is 200W, and ultrasonic frequency is 60KHZ, and the ultrasonic oscillation time is 1～3h; Subsequently mixing solutions is carried out to centrifugal purification processing, described centrifugal rotational speed is 4000rpm～12000rpm, and centrifugation time is 1～30min; Preferably centrifugation time is 10～20min.
7. the preparation method of a kind of Graphene spray according to claim 4, is characterized in that: the solvent in described step 2 is the mixture of water or organic solvent or at least two kinds of organic solvents; Described organic solvent is methyl alcohol or ethanol or Virahol or acetone or ethyl acetate or chloroform or tetracol phenixin or tetrahydrofuran (THF) or DMF or dimethyl sulfoxide (DMSO) or benzene or toluene or dimethylbenzene or chlorobenzene or dichlorobenzene or trichlorobenzene; Preferred solvent is one or any two or more the mixture of organic solvent in water, methyl alcohol, ethanol, acetone, ethyl acetate, chloroform, tetrahydrofuran (THF), benzene, toluene.
8. the preparation method of a kind of Graphene spray according to claim 4, is characterized in that: the graphene solution concentration obtaining in described step 2 is 0.5～15mg/ml.
9. the application of Graphene spray according to claim 1, it is characterized in that: with Graphene spray, outdoor goods surface is carried out the purposes of waterproof and breathable processing, by direct articles for use out of doors surface after outdoor goods surface spraying being formed to the graphene film of waterproof and breathable.
10. the application of Graphene spray according to claim 9, is characterized in that: the thickness of the graphene film that after described spraying, articles for use surface forms is out of doors 0.1～100 μ m; Be preferably 1～80 μ m, more preferably 5～60 μ m, most preferably are 10～50 μ m.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110699948A (en) * | 2019-10-30 | 2020-01-17 | 武汉低维材料研究院有限公司 | Tin oxide/silver nanowire/graphene electronic textile and preparation method thereof |
| CN113355908A (en) * | 2021-03-19 | 2021-09-07 | 广州市奥因环保科技有限公司 | Multifunctional antibacterial and deodorant textile knitwear and preparation method and production device thereof |
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| CN102040797A (en) * | 2010-12-28 | 2011-05-04 | 哈尔滨工业大学 | Graphene/TiO2-based near-infrared/ultraviolet radiation resistant polymer composite film and preparation method thereof |
| CN102500287A (en) * | 2011-09-28 | 2012-06-20 | 重庆大学 | Graphene/modified titanium dioxide nano sol composite material and preparation method thereof |
| CN103806266A (en) * | 2013-11-25 | 2014-05-21 | 江南大学 | Method for manufacturing graphene oxide conductive cellulose fabric by ultraviolet light |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101474899A (en) * | 2009-01-16 | 2009-07-08 | 南开大学 | Grapheme-organic material layered assembling film and preparation method thereof |
| CN102040797A (en) * | 2010-12-28 | 2011-05-04 | 哈尔滨工业大学 | Graphene/TiO2-based near-infrared/ultraviolet radiation resistant polymer composite film and preparation method thereof |
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| CN103806266A (en) * | 2013-11-25 | 2014-05-21 | 江南大学 | Method for manufacturing graphene oxide conductive cellulose fabric by ultraviolet light |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110699948A (en) * | 2019-10-30 | 2020-01-17 | 武汉低维材料研究院有限公司 | Tin oxide/silver nanowire/graphene electronic textile and preparation method thereof |
| CN113355908A (en) * | 2021-03-19 | 2021-09-07 | 广州市奥因环保科技有限公司 | Multifunctional antibacterial and deodorant textile knitwear and preparation method and production device thereof |
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Application publication date: 20140813 |