CN104212413B - A kind of ice-covering-proof material of liquid filling cellular silicone and preparation method - Google Patents
A kind of ice-covering-proof material of liquid filling cellular silicone and preparation method Download PDFInfo
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- CN104212413B CN104212413B CN201410475514.2A CN201410475514A CN104212413B CN 104212413 B CN104212413 B CN 104212413B CN 201410475514 A CN201410475514 A CN 201410475514A CN 104212413 B CN104212413 B CN 104212413B
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- 229920001296 polysiloxane Polymers 0.000 title claims abstract description 136
- 230000001413 cellular effect Effects 0.000 title claims abstract description 132
- 239000007788 liquid Substances 0.000 title claims abstract description 129
- 239000000463 material Substances 0.000 title claims abstract description 103
- 238000011049 filling Methods 0.000 title claims abstract description 69
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000011737 fluorine Substances 0.000 claims abstract description 58
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 58
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 55
- 239000002105 nanoparticle Substances 0.000 claims abstract description 50
- 238000002156 mixing Methods 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000007711 solidification Methods 0.000 claims abstract description 16
- 230000008023 solidification Effects 0.000 claims abstract description 16
- 239000002245 particle Substances 0.000 claims abstract description 15
- 239000002904 solvent Substances 0.000 claims abstract description 15
- 230000004048 modification Effects 0.000 claims abstract description 12
- 238000012986 modification Methods 0.000 claims abstract description 12
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 12
- 239000010703 silicon Substances 0.000 claims abstract description 12
- 239000003054 catalyst Substances 0.000 claims abstract description 11
- ZHPNWZCWUUJAJC-UHFFFAOYSA-N fluorosilicon Chemical compound [Si]F ZHPNWZCWUUJAJC-UHFFFAOYSA-N 0.000 claims abstract description 11
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000758 substrate Substances 0.000 claims abstract description 10
- 239000002131 composite material Substances 0.000 claims abstract description 4
- 238000007385 chemical modification Methods 0.000 claims description 34
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 24
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 21
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 16
- -1 fluorine octyl group Trimethoxy silanes Chemical class 0.000 claims description 16
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 14
- 238000002679 ablation Methods 0.000 claims description 14
- 239000010949 copper Substances 0.000 claims description 14
- 229910052802 copper Inorganic materials 0.000 claims description 14
- 239000011521 glass Substances 0.000 claims description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 13
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 229910052742 iron Inorganic materials 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 239000004793 Polystyrene Substances 0.000 claims description 11
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 11
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 11
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 11
- 229920002223 polystyrene Polymers 0.000 claims description 11
- 239000010936 titanium Substances 0.000 claims description 11
- 229910052719 titanium Inorganic materials 0.000 claims description 11
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 10
- 229920000747 poly(lactic acid) Polymers 0.000 claims description 10
- 229910000077 silane Inorganic materials 0.000 claims description 10
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 8
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 8
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 7
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 7
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- 238000004090 dissolution Methods 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 6
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 6
- ZUEKXCXHTXJYAR-UHFFFAOYSA-N tetrapropan-2-yl silicate Chemical compound CC(C)O[Si](OC(C)C)(OC(C)C)OC(C)C ZUEKXCXHTXJYAR-UHFFFAOYSA-N 0.000 claims description 6
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 5
- LLGVQQLZYJJDBZ-UHFFFAOYSA-N trimethoxy(2,2,2-trifluoroethyl)silane Chemical compound CO[Si](OC)(OC)CC(F)(F)F LLGVQQLZYJJDBZ-UHFFFAOYSA-N 0.000 claims description 5
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- 239000001913 cellulose Substances 0.000 claims description 4
- 229920002678 cellulose Polymers 0.000 claims description 4
- 235000019253 formic acid Nutrition 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 4
- 238000005507 spraying Methods 0.000 claims description 4
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 claims description 4
- OAIHZBDIHWTNRB-UHFFFAOYSA-N 1,1,2,4,4,4-hexafluorobutyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C(F)(F)C(F)CC(F)(F)F OAIHZBDIHWTNRB-UHFFFAOYSA-N 0.000 claims description 3
- FBCRWVBKSFQUFF-UHFFFAOYSA-N [F].CCCCCCCC[Si](OCC)(OCC)OCC Chemical compound [F].CCCCCCCC[Si](OCC)(OCC)OCC FBCRWVBKSFQUFF-UHFFFAOYSA-N 0.000 claims description 3
- 235000019353 potassium silicate Nutrition 0.000 claims description 3
- YCCWZUJLIHFITJ-UHFFFAOYSA-N triethoxy(1,1,2,4,4,4-hexafluorobutyl)silane Chemical compound FC(C([Si](OCC)(OCC)OCC)(F)F)CC(F)(F)F YCCWZUJLIHFITJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 239000004411 aluminium Substances 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 239000011260 aqueous acid Substances 0.000 claims description 2
- 238000007654 immersion Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 17
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- 229910019142 PO4 Inorganic materials 0.000 description 2
- PRPAGESBURMWTI-UHFFFAOYSA-N [C].[F] Chemical compound [C].[F] PRPAGESBURMWTI-UHFFFAOYSA-N 0.000 description 2
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- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
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- 238000003682 fluorination reaction Methods 0.000 description 1
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- NOBMQPILAFKJLD-UHFFFAOYSA-N triethoxy(2,2,2-trifluoroethyl)silane Chemical compound CCO[Si](CC(F)(F)F)(OCC)OCC NOBMQPILAFKJLD-UHFFFAOYSA-N 0.000 description 1
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- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Paints Or Removers (AREA)
- Laminated Bodies (AREA)
Abstract
A kind of ice-covering-proof material of liquid filling cellular silicone and preparation method.Base material of the present invention combines by the cellular silicone of silicon fluoride modification and fluorine-containing liquid composite bed, wherein, fluorine-containing liquid filling is in the cellular silicone of silicon fluoride modification; Cellular silicone to be mixed in a solvent with organic nano particle by inorganic silicon or organosilicon materials, catalyst solution and forms mixing solutions, is directly coated in substrate surface, removes organic nano particle and obtain after solidification to be dried; Described fluorine-containing liquid be selected from liquid fluorocarbon, liquid fluorine silicon one or both; Described fluorine-containing liquid range of viscosities is at room temperature 0.1 ~ 500cm
2/ s; The average particle size range of described organic nano particle is 50 ~ 800nm.When envrionment temperature and ambient moisture can cause base material to freeze, described liquid filling cellular silicone surface can stop supercooled water contact substrate, liquid lubrication layer also can make the adhesive power of ice sheet significantly decline, and easily under gravity or wind effect, departs from surface.It is 0 DEG C ~-40 DEG C that material of the present invention efficiently can act on envrionment temperature, and ambient moisture is the weather condition such as 40% ~ 90%.
Description
Technical field
The invention belongs to field of material technology, be specifically related to ice-covering-proof material of a kind of liquid filling cellular silicone and preparation method thereof.
Background technology
Icing phenomenon is very common at occurring in nature, is present in the surface of various low temperature widely, and as the open air of Cold Winter and the evaporator surface of various refrigeration system and refrigerating apparatus, icing brings all multiple-energy-sources and safety problem.Such as: icing can cause refrigerating apparatus heat transfer efficiency to decline to a great extent even losing efficacy; Aircraft can be caused in the air to crash for serious icing and ecotope, traffic, electric power facility is by considerable damage etc.Usually, ice detachment needs human and material resources and the financial resources of at substantial.Therefore, how effectively to solve or alleviate the icing problem of cold surface, reduce anti-icing energy consumption and the hot issue becoming anti-icing research field avoiding security incident.Existing ice-covering-proof technology mainly contains heating power deicing, several classes such as manual machine deicing and ice-covering-proof material.Wherein, the energy consumption of heating power deicing is large, and manual machine deicing efficiency is low, potential safety hazard is large.Ice-covering-proof material fundamentally can prevent material surface from freezing or reduce icing degree, is the Perfected process solving icing problem, thus receives much attention.
At present, the anti-icing main policies of material comes ice-covering-proof by constructing special wetting property surface, comprises two classes: a class is hydrophilic surface, utilize the large water gaging of absorbing hydrophilic materials, and add and can fall subzero material (CN1104674A, CN1632014A, CN1916094A).But the water regain of this kind of material and rate of water absorption are very large to anti-icing influential effect, weak effect under the environment of high humidity, consecutive low temperature, and fall subzero material and generally select small-molecule substance, easily run off, work-ing life is limited.Another kind of is water repellent surface, reduces heat transfer efficiency by minimizing water droplet and contact surface area, delays water droplet and freezes (CN1556161A, CN102660182A).But its hydrophobic performance is large to anti-icing influential effect, and can not reduce the adhesive power of ice on surface.Also have the anti-icing method adopting compound surface, patent CN100593557C mixes hydrophilic with hydrophobic polymer, utilizes phase detachment technique to obtain the composite structure of strong hydrophilicity internal layer and super hydrophobic surface, achieves good anti-icing effect.
Liquid surface layer is adopted to intercept the contact of ice sheet and base material and reduce adhesive power technology (the Wong T.S of ice sheet; KangS.H.; Tang S.K.Y.; Smythe E.J.; Hatton B.D.; Grinthal A.; Aizenberg J.Nature2011,477,443-447) in.The key on this surface is at surface construction one deck liquid surface layer, usually utilizes the capillary force of porous epoxy resin or fluorinated polymer material and liquid to keep liquid.Common vesicular structure preparation method comprises Lithographic template method, reversion colloid crystallization, microphase-separated method etc., these methods or need specific installation, or preparation method is numerous and diverse, or high to material selectivity, is not suitable for industrialized practical application.
Summary of the invention
The object of the present invention is to provide the ice-covering-proof material of a kind of low ice adhesion liquid filling cellular silicone.
Another object of the present invention is to provide a kind of low ice adhesion liquid filling cellular silicone ice-covering-proof material preparation method.
The ice-covering-proof material of liquid filling cellular silicone of the present invention, base material combines by the cellular silicone of silicon fluoride modification and fluorine-containing liquid composite bed, wherein, fluorine-containing liquid filling is in the cellular silicone of silicon fluoride modification; Cellular silicone to be mixed in a solvent with organic nano particle by inorganic silicon or organosilicon materials, catalyst solution and forms mixing solutions, is directly coated in substrate surface, removes organic nano particle and obtain after solidification to be dried; Described fluorine-containing liquid is selected from one or more in liquid fluorocarbon, liquid fluorine silicon; Described fluorine-containing liquid range of viscosities is at room temperature 0.1 ~ 500cm
2/ s; The average particle size range of described organic nano particle is 50 ~ 800nm.
The cellular silicone of silicon fluoride modification is joined by the base material being coated with cellular silicone in the encloses container being placed with silicon fluoride or immerse to be dissolved with in the solution of fluorine containing silane to carry out surface chemical modification and form.
The ice-covering-proof material of liquid filling cellular silicone of the present invention can make the adhesive power of ice and base material significantly reduce.The ice-covering-proof material of liquid filling cellular silicone of the present invention is composited by the cellular silicone of silicon fluoride modification and fluorine-containing liquid.
Described silicon fluoride is selected from one or more in trifluoroethyl Trimethoxy silane, trifluoroethyl Trimethoxy silane, hexafluoro butyl trimethoxy silane, hexafluoro butyl triethoxyl silane, five fluorine octyl group Trimethoxy silanes, five fluorine octyltri-ethoxysilane, perfluoro capryl Trimethoxy silane, perfluoro capryl triethoxy.
Described inorganic silicon raw material is water glass.Organosilicon materials is selected from one or more in methyl silicate, tetraethoxy or positive isopropyl silicate.
Described catalyst solution is aqueous acid.Described acid is selected from one or more in hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, formic acid, aqueous acetic acid.Described catalyst solution concentration range is 0.01 ~ 1mol/L.The volume ratio of catalyst solution and mixing solutions is 1:10 ~ 1:100.
Described organic nano particle is selected from one or more in polystyrene, polymethylmethacrylate, polyacrylonitrile, polylactide, poly(lactic acid), nano-cellulose.
Solvent in described mixing solutions is selected from one or more in water, methyl alcohol, ethanol, propyl alcohol, Virahol, butanols, acetone.
Contriver by further studying discovery, because both the viscosity of fluorine-containing liquid and organic nano particle have synergistic function, all can have impact to anti-icing performance.
Research of the present invention also shows, the viscosity of fluorine-containing liquid is preferably 0.1 ~ 50cm
2/ s; The particle size range of organic nano particle is preferably 200 ~ 500nm, can obtain the effect of best low ice adhesion.
The preparation method of the ice-covering-proof material of liquid filling cellular silicone provided by the invention, comprise the steps: the preparation of (1) cellular silicone: organic nano particle is joined massfraction be 10% ~ 50% inorganic silicon or organic silicon solution in, after mixing, add catalyst solution, the mixing solutions formed directly is coated in substrate surface, and after solidification to be dried, high temperature ablation or dissolution with solvents are removed organic nano particle and obtained cellular silicone surface.
(2) cellular silicone surface chemical modification: the encloses container having cellular silicone base material to be placed on surface obtained to (1) to be placed with silicon fluoride or immerse the solution being dissolved with fluorine containing silane and carry out surface chemical modification.
(3) fluorine-containing liquid filling: adopt the methods such as spraying or immersion to be fixed in the cellular silicone of surface chemical modification by fluorine-containing liquid.
The mass ratio of described organic nano particle and inorganic silicon or organosilicon materials is 1:1 ~ 1:4.
The method of described removal organic nano particle comprises high temperature ablation or dissolution with solvents.
The temperature province of described high temperature ablation is selected from 300 ~ 800 DEG C.The ablation time is selected from 30 ~ 1200min.
One or more in the solvent selected from chloroform that the method for described dissolution with solvents uses, methylene dichloride, tetracol phenixin, tetrahydrofuran (THF), dimethyl formamide.Soak time is selected from 2 ~ 24h.
The time of described surface chemical modification is 2 ~ 48h.
One or more in solvent selected from methanol in the solution of fluorine containing silane, ethanol, acetone, benzene, chloroform.In described fluorine containing silane solution, the massfraction of silicon fluoride is 1% ~ 20%.
The application of the ice-covering-proof material of liquid filling cellular silicone of the present invention, can on different base materials preparation liquid filling cellular silicone surface, obtain that there is low ice and adhere to ice-covering-proof material.
When envrionment temperature and ambient moisture can cause base material to freeze, described liquid filling cellular silicone surface can stop supercooled water contact substrate, liquid lubrication layer also can make the adhesive power of ice sheet significantly decline, and easily under gravity or wind effect, departs from surface.It is 0 DEG C ~-40 DEG C that material of the present invention efficiently can act on envrionment temperature, and ambient moisture is the weather condition such as 40% ~ 90%.
Described base material can be copper, iron, aluminium, titanium, glass, pottery etc.
The invention provides the ice-covering-proof material of a kind of liquid filling cellular silicone.This surface to be mixed with organic nano particle by inorganic silicon conventional in industrial production or organosilicon materials and is directly coated in substrate surface, go organic nano particle namely to obtain cellular silicone after solidification to be dried, then obtain ice-covering-proof material through surface fluorination and modification and the non-volatile hydrophobic liquid of filling.Wherein non-volatile hydrophobic liquid effectively can be fixed on surface by the cellular silicone of surface modification, thus forms one deck liquid surface layer.
The ice-covering-proof material of liquid filling cellular silicone of the present invention has the following advantages compared to other ice-covering-proof material: the ice adhesion that (1) is ultralow: due to the present invention formed can ice-covering-proof effect have isolation and the fluorine containing silane modified liquid layer of lubrication concurrently, both the formation of ice sheet can have been delayed, ice and substrate adhesive power can be greatly reduced again, make substrate surface icing less and easily remove under wind-force and action of gravity.The adhesive power of material of the present invention can remain on below 100kPa substantially, and wherein embodiment 1-4 can remain on below 50kPa, see Fig. 1,2.Specifically can be further, compared to various unmodified base material, see Fig. 3, can find out, the ice adhesion of base material is at least more than 800Kpa.Therefore, the ice-covering-proof material of liquid filling cellular silicone prepared by the present invention is carrying out modification to cellular silicone, all show good ice-covering-proof ability in conjunction with resulting materials on the basis of the comprehensive action of organic nano particle and fluorine-containing liquid viscosity, ice adhesion obviously weakens simultaneously.Illustrate that material surface and ice sheet have been carried out good isolation by the liquid filling cellular silicone in the present invention program, its lubrication also makes ice adhesion obviously decline.Simultaneously, comparison diagram 1 and Fig. 2, can find out the ice-covering-proof material (embodiment 5 ~ 8) that ice adhesion is less than the fluorine-containing liquid of high viscosity, prepared by small particle size/Large stone organic nano particle of ice-covering-proof material (embodiment 1 ~ 4) prepared by the organic nano particle selecting the fluorine-containing liquid-mixing of more low viscosity to unify to determine particle diameter.In conjunction with comparative example 9 and 10, in the present invention, fluorine-containing fitting of fluids scope is 0.1 ~ 500cm
2/ s, is preferably 0.1 ~ 50cm
2/ s, organic nano particle particle diameter range of choice is 50 ~ 800nm, is preferably 200 ~ 500nm.(2) wearing quality is strong: the present invention uses silicone material, satisfactory mechanical property; The fluorine-containing liquid stability used is good, and environmental resistance ability is strong, and fluorine-containing material surface energy is low, is not easy contaminated; Flowing fluid layer can also repair local damage.
Accompanying drawing illustrates:
Fig. 1. the ice-covering-proof material of liquid filling cellular silicone prepared of the embodiment of the present invention 1 ~ 4 envrionment temperature be-20 DEG C, ambient moisture is 60%, after freezing 12 hours, carries out the result of ice adhesion size test.
Fig. 2. the ice-covering-proof material of liquid filling cellular silicone prepared of embodiment 5 ~ 8 envrionment temperature be-40 DEG C, ambient moisture is 90%, carries out the result of ice adhesion size test after freezing 12 hours.
Fig. 3. various unmodified base material envrionment temperature be 0 DEG C, ambient moisture is 40%, after freezing 12 hours, carries out the result of ice adhesion size test.
Fig. 4. the silicone surface SEM photo of (b) after dry solidification (a) and intensification ablation in embodiment 1.
Fig. 5. select particle diameter to be silicone surface SEM photo prepared by 20nm and 1000nm polystyrene nanoparticle in comparative example 9.
Fig. 6. the ice-covering-proof material of liquid filling cellular silicone of comparative example 10 envrionment temperature be 0 DEG C, ambient moisture is 40%, after freezing 12 hours, carries out the result of ice adhesion size test.
Embodiment
Below by way of specific embodiment, the present invention is described, but embodiment only for illustration of, do not limit the scope of the invention.When not departing from aforesaid method thought range of the present invention, the various replacement made according to ordinary skill knowledge and customary means and change, all should be within the scope of the present invention.
The experimental technique used in following embodiment if no special instructions, is ordinary method.
Material used in following embodiment, reagent etc., if no special instructions, all can obtain from commercial channels.
Embodiment 1
(1) preparation of cellular silicone
The polystyrene nanoparticle (median size is 500nm) of certain mass being joined massfraction is (mass ratio of polystyrene and water glass is 1:1) in the sodium silicate aqueous solution of 10%, after mixing, add the aqueous hydrochloric acid (aqueous hydrochloric acid and mixed liquor volume are than being 1:20) of 0.1mol/L, then solution is directly coated in copper sheet surface, after solution dry solidification, put into retort furnace be warming up to 800 DEG C of ablation 30min, take out copper sheet after cooling and obtain the copper sheet that there is cellular silicone on surface.
(2) cellular silicone surface chemical modification
There is the copper sheet of cellular silicone to be placed on surface obtained for step (1) to be placed with the encloses container 24h of trifluoroethyl Trimethoxy silane, obtain the copper sheet of the cellular silicone of surface chemical modification.
Fig. 4 shows that nanoparticle is evenly dispersed in silicone resin, reunites in film forming and dry solidification process.In intensification ablation process, in silicone resin, organic nano particle is removed, and defines vesicular structure, and pore structure is even, and non-occurrence of large-area is caved in and empty structure.
(3) fluorine-containing liquid filling
Be 0.1cm by viscosity
2on the copper sheet that the method even application of the fluorocarbon liquid spraying of/s covers to the cellular silicone of the obtained surface chemical modification of step (2), the ice-covering-proof material of acquisition liquid filling cellular silicone.
When envrionment temperature is 0 ~-40 DEG C, ambient moisture be 40% ~ 90% can cause copper sheet surface freeze time, the above-mentioned obtained ice-covering-proof material of liquid filling cellular silicone can stop supercooled water to contact copper sheet, copper sheet surface is frozen reduce and the adhesive power of ice sheet reduces greatly, the ice sheet on copper sheet surface can depart under the effect of gravity or wind-force.
Embodiment 2
(1) preparation of cellular silicone
The polymethyl methacrylate nano particle (median size is 400nm) of certain mass being joined massfraction is (mass ratio of polymethylmethacrylate and methyl silicate is 1:2) in the methyl silicate/methanol solution of 20%, after mixing, add the aqueous sulfuric acid (aqueous sulfuric acid and mixed liquor volume are than being 1:10) of 0.3mol/L, then solution is directly coated in iron plate surface, after solution dry solidification, put into retort furnace be warming up to 300 DEG C of ablation 1200min, take out iron plate after cooling and obtain the iron plate that there is cellular silicone on surface.
(2) cellular silicone surface chemical modification
There is the copper sheet of cellular silicone to be placed on surface obtained for step (1) to be placed with the encloses container 48h of trifluoroethyl triethoxyl silane, obtain the iron plate of the cellular silicone of surface chemical modification.
(3) fluorine-containing liquid filling
Be 50cm by viscosity
2on the iron plate that the method even application of the fluorocarbon liquid spraying of/s covers to the cellular silicone of the obtained surface chemical modification of step (2), the ice-covering-proof material of acquisition liquid filling cellular silicone.
When envrionment temperature is 0 ~-40 DEG C, ambient moisture be 40% ~ 90% can cause iron plate surface freeze time, the above-mentioned obtained ice-covering-proof material of liquid filling cellular silicone can stop supercooled water to contact iron plate, iron plate surface is frozen reduce and the adhesive power of ice sheet reduces greatly, the ice sheet on iron plate surface can depart under the effect of gravity or wind-force.
Embodiment 3
(1) preparation of cellular silicone
The nano-cellulose (median size is 300nm) of certain mass being joined massfraction is (mass ratio of nano-cellulose and tetraethoxy is 1:4) in the tetraethoxy/ethanolic soln of 40%, after mixing, add the aqueous nitric acid (aqueous nitric acid and mixed liquor volume are than being 1:30) of 0.5mol/L, then solution is directly coated in glass sheet surface, after solution dry solidification, put into retort furnace be warming up to 500 DEG C of ablation 800min, take out iron plate after cooling and obtain the sheet glass that there is cellular silicone on surface.
(2) cellular silicone surface chemical modification
Have the sheet glass of cellular silicone to be soaked in massfraction on the surface that step (1) is obtained to be 6h in the methanol solution of the hexafluoro butyl trimethoxy silane of 1%, to obtain the sheet glass of the cellular silicone of surface chemical modification.
(3) fluorine-containing liquid filling
It is 1cm that the sheet glass that the cellular silicone of surface chemical modification obtained for step (2) covers is dipped into viscosity
2in the fluorine silicon solution of/s, then take out the fluorine silicon liquid wiping excess surface away, obtain the ice-covering-proof material of liquid filling cellular silicone.
When envrionment temperature is 0 ~-40 DEG C, ambient moisture is 40% ~ 90% when glass sheet surface can be caused to freeze, the above-mentioned obtained ice-covering-proof material of liquid filling cellular silicone can stop supercooled water to contact sheet glass, freeze minimizing and the adhesive power of ice sheet of glass sheet surface is reduced greatly, and the ice sheet of glass sheet surface can depart under the effect of gravity or wind-force.
Embodiment 4
(1) preparation of cellular silicone
The polyacrylonitrile nano particle (median size is 200nm) of certain mass being joined massfraction is (mass ratio of polyacrylonitrile and positive isopropyl silicate is 1:4) in the positive isopropyl silicate/propanol solution of 50%, after mixing, add the phosphate aqueous solution (phosphate aqueous solution and mixed liquor volume are than being 1:100) of 0.8mol/L, then solution is directly coated in aluminium flake surface, after solution dry solidification, immerses 12h in tetrahydrofuran (THF) remove the aluminium flake that there is cellular silicone on polyacrylonitrile nano particle acquisition surface.
(2) cellular silicone surface chemical modification
Have the aluminium flake of cellular silicone to be soaked in massfraction on the surface that step (1) is obtained to be 48h in the methanol solution of the hexafluoro butyl triethoxyl silane of 5%, to obtain the aluminium flake of the cellular silicone of surface chemical modification.
(3) fluorine-containing liquid filling
It is 30cm that the aluminium flake that the cellular silicone of surface chemical modification obtained for step (2) covers is dipped into viscosity
2in the fluorine silicon liquid of/s, then take out the fluorine silicon liquid wiping excess surface away, obtain the ice-covering-proof material of liquid filling cellular silicone.
When envrionment temperature is 0 ~-40 DEG C, ambient moisture be 40% ~ 90% can cause aluminium flake surface freeze time, the above-mentioned obtained ice-covering-proof material of liquid filling cellular silicone can stop supercooled water to contact aluminium flake, aluminium flake surface is frozen reduce and the adhesive power of ice sheet reduces greatly, the ice sheet on aluminium flake surface can depart under the effect of gravity or wind-force.
Embodiment 5
(1) preparation of cellular silicone
The polylactide nanoparticles (median size is 600nm) of certain mass being joined massfraction is (mass ratio of polylactide and tetraethoxy is 1:3) in the tetraethoxy/aqueous isopropanol of 50%, after mixing, add the aqueous formic acid (aqueous formic acid and mixed liquor volume are than being 1:100) of 1mol/L, then solution is directly coated in titanium plate surface, after solution dry solidification, immerses 12h in chloroform remove the titanium sheet that there is cellular silicone on polylactide nanoparticles acquisition surface.
(2) cellular silicone surface chemical modification
Have the titanium sheet of cellular silicone to be soaked in massfraction on the surface that step (1) is obtained to be 2h in the ethanolic soln of the five fluorine octyl group Trimethoxy silanes of 10%, to obtain the titanium sheet of the cellular silicone of surface chemical modification.
(3) fluorine-containing liquid filling
It is 300cm that the titanium sheet that the cellular silicone of surface chemical modification obtained for step (2) covers is dipped into viscosity
2in the fluorine silicon solution of/s, then take out the fluorine silicon liquid wiping excess surface away, obtain the ice-covering-proof material of liquid filling cellular silicone.
When envrionment temperature is 0 ~-40 DEG C, ambient moisture is 40% ~ 90% when titanium plate surface can be caused to freeze, the above-mentioned obtained ice-covering-proof material of liquid filling cellular silicone can stop supercooled water to contact titanium sheet, freeze minimizing and the adhesive power of ice sheet of titanium plate surface is reduced greatly, and the ice sheet of titanium plate surface can depart under the effect of gravity or wind-force.
Embodiment 6
(1) preparation of cellular silicone
The nano polylactic acid particle (median size is 150nm) of certain mass being joined massfraction is (mass ratio of poly(lactic acid) and positive isopropyl silicate is 1:2) in the positive isopropyl silicate/butanol solution of 20%, after mixing, add the acetic acid aqueous solution (acetic acid aqueous solution and mixed liquor volume are than being 1:60) of 0.2mol/L, then solution is directly coated in ceramic plate surface, after solution dry solidification, immerses 2h in benzene remove the ceramic plate that there is cellular silicone on nano polylactic acid particle acquisition surface.
(2) cellular silicone surface chemical modification
Have the ceramic plate of cellular silicone to be soaked in massfraction on the surface that step (1) is obtained to be 10h in the acetone soln of the five fluorine octyltri-ethoxysilane of 15%, to obtain the ceramic plate of the cellular silicone of surface chemical modification.
(3) fluorine-containing liquid filling
It is 500cm that the ceramic plate that the cellular silicone of surface chemical modification obtained for step (2) covers is dipped into viscosity
2in the fluorine carbon solution of/s, then take out the fluorocarbon liquid wiping excess surface away, obtain the ice-covering-proof material of liquid filling cellular silicone.
When envrionment temperature is 0 ~-40 DEG C, ambient moisture be 40% ~ 90% can cause ceramic plate surface freeze time, the above-mentioned obtained ice-covering-proof material of liquid filling cellular silicone can stop supercooled water to contact ceramic plate, ceramic plate surface is frozen reduce and the adhesive power of ice sheet reduces greatly, the ice sheet on ceramic plate surface can depart under the effect of gravity or wind-force.
Embodiment 7
(1) preparation of cellular silicone
The polystyrene nanoparticle (median size is 800nm) of certain mass being joined massfraction is (mass ratio of polystyrene and methyl silicate is 1:3) in the methyl silicate/aqueous solution of 8%, after mixing, add the aqueous hydrochloric acid (aqueous hydrochloric acid and mixed liquor volume are than being 1:30) of 1mol/L, then solution is directly coated in glass sheet surface, after solution dry solidification, immerses 4h in tetrahydrofuran (THF) remove the ceramic plate that there is cellular silicone on polystyrene nanoparticle acquisition surface.
(2) cellular silicone surface chemical modification
Have the sheet glass of cellular silicone to be soaked in massfraction on the surface that step (1) is obtained to be 15h in the acetone soln of the perfluoro capryl Trimethoxy silane of 6%, to obtain the sheet glass of the cellular silicone of surface chemical modification.
(3) fluorine-containing liquid filling
It is 100cm that the sheet glass that the cellular silicone of surface chemical modification obtained for step (2) covers is dipped into viscosity
2in the fluorine carbon solution of/s, then take out the fluorocarbon liquid wiping excess surface away, obtain the ice-covering-proof material of liquid filling cellular silicone.
When envrionment temperature is 0 ~-40 DEG C, ambient moisture is 40% ~ 90% when glass sheet surface can be caused to freeze, the above-mentioned obtained ice-covering-proof material of liquid filling cellular silicone can stop supercooled water to contact sheet glass, freeze minimizing and the adhesive power of ice sheet of glass sheet surface is reduced greatly, and the ice sheet of glass sheet surface can depart under the effect of gravity or wind-force.
Embodiment 8
(1) preparation of cellular silicone
The polymethyl methacrylate nano particle (median size is 50nm) of certain mass being joined massfraction is (mass ratio of polymethylmethacrylate and tetraethoxy is 1:1) in the tetraethoxy/propanol solution of 12%, after mixing, add the aqueous nitric acid (aqueous nitric acid and mixed liquor volume are than being 1:20) of 0.6mol/L, then solution is directly coated in glass sheet surface, after solution dry solidification, immerses 4h in chloroform remove the ceramic plate that there is cellular silicone on polymethyl methacrylate nano particle acquisition surface.
(2) cellular silicone surface chemical modification
Have the sheet glass of cellular silicone to be soaked in massfraction on the surface that step (1) is obtained to be 15h in the chloroformic solution of the perfluoro capryl Trimethoxy silane of 8%, to obtain the sheet glass of the cellular silicone of surface chemical modification.
(3) fluorine-containing liquid filling
It is 500cm that the sheet glass that the cellular silicone of surface chemical modification obtained for step (2) covers is dipped into viscosity
2in the fluorine silicon solution of/s, then take out the fluorocarbon liquid wiping excess surface away, obtain the ice-covering-proof material of liquid filling cellular silicone.
When envrionment temperature is 0 ~-40 DEG C, ambient moisture is 40% ~ 90% when glass sheet surface can be caused to freeze, the above-mentioned obtained ice-covering-proof material of liquid filling cellular silicone can stop supercooled water to contact sheet glass, freeze minimizing and the adhesive power of ice sheet of glass sheet surface is reduced greatly, and the ice sheet of glass sheet surface can depart under the effect of gravity or wind-force.
Comparative example 9
In the ice-covering-proof material preparation of liquid filling cellular silicone of the present invention, the first step is prepared cellular silicone and is selected the scope of organic nano particle to be 50 ~ 800nm.For the necessity that checking organic nano particle particle diameter of the present invention is selected, this comparative example, according to the preparation process of embodiment 1, prepares cellular silicone and selects the polystyrene nanoparticle that the scope use median size of organic nano particle is 20nm and 1000nm to prepare liquid filling cellular silicone on copper sheet surface.
Fig. 5 is the silicone surface SEM photo selecting 20nm (a) and 1000nm (b) polystyrene nanoparticle to prepare in comparative example 9.
No matter the polystyrene nanoparticle being 20nm or 1000nm is all undesirable for the preparation of the result of cellular silicone.When particle diameter is too small, because nanoparticle is embedded in silicone resin completely, form unicellular structure after ablation, hole almost be can't see in surface.Liquid film can not be formed on surface at the fluorine-containing liquid of liquid compound tense like this, anti-icing function cannot be realized.In the comparative example that particle diameter is excessive, can see that surface is except forming the hole close with nano particle diameter size, yet forms both big area defect.Because fluorine-containing liquid main capillary force that relies in pore structure is fixed, defect can cause the fluorine-containing unstabilizing liquid in this region, and the liquid surface layer of formation is imperfect.Therefore, this structure is also disadvantageous to fluorine-containing liquid again, easily forms ice and adheres to concentrated area, make anti-icing degradation.Therefore, experimentally and analyze, in the present invention, the particle size range of nanoparticle is chosen as 50 ~ 800nm.
Comparative example 10
In the ice-covering-proof material preparation of liquid filling cellular silicone of the present invention, contriver examines the viscosity of fluorine-containing liquid further on the impact of material anti-icing performance, and liquid volatile is on the impact of the long-acting usability of material.Because fluorine-containing liquid viscosity is relevant to its molecular weight, viscosity is lower than 0.1cm
2the fluorine-containing liquid of/s is small-molecule substance, has obvious volatility, and the fluorine-containing liquid viscosity therefore selected in the present invention is greater than 0.1cm
2/ s.In this comparative example, according to the preparation process of embodiment 1, employ viscosity from 0.1cm
2/ s ~ 1000cm
2the fluorocarbon liquid of/s is as the filling liquid of step (3).
Fig. 6 be comparative example 10 the ice-covering-proof material of liquid filling cellular silicone envrionment temperature be 0 DEG C, ambient moisture is 40%, after freezing 12 hours, carries out the result of the test of ice adhesion size.
In Fig. 6, ice sheet adhesive power has different-effect along with the rising of viscosity.(<50cm within the scope of low viscosity
2/ s), ice-covering-proof material adhesion minimum (<50KPa) prepared by fluorocarbon liquid and fluorine silicon liquid, ice-covering-proof effect is excellent.(50 ~ 500cm within the scope of medium-viscosity
2/ s), ice-covering-proof material adhesion prepared by fluorine-containing liquid also less (<100KPa), has good ice-covering-proof ability.But, but the viscosity of fluorine-containing liquid is more than 500cm
2after/s, the ice-covering-proof successful of material declines (ice adhesion >145KPa).Therefore, the range of viscosities of the fluorine-containing liquid selected in the present invention is 0.1 ~ 500cm
2/ s, preferable range is 0.1 ~ 50cm
2/ s.
Claims (15)
1. the ice-covering-proof material of liquid filling cellular silicone, is characterized in that: base material combines by the cellular silicone of silicon fluoride modification and fluorine-containing liquid composite bed, wherein, fluorine-containing liquid filling is in the cellular silicone of silicon fluoride modification; Cellular silicone to be mixed in a solvent with organic nano particle by inorganic silicon or organosilicon materials, catalyst solution and forms mixing solutions, is directly coated in substrate surface, removes organic nano particle and obtain after solidification to be dried; Described fluorine-containing liquid be selected from liquid fluorocarbon, liquid fluorine silicon one or both; Described fluorine-containing liquid range of viscosities is at room temperature 0.1 ~ 500 cm
2/ s; The average particle size range of described organic nano particle is 50 ~ 800 nm.
2. the ice-covering-proof material of liquid filling cellular silicone according to claim 1, is characterized in that: described fluorine-containing liquid range of viscosities is at room temperature 0.1 ~ 50cm
2/ s; The average particle size range of described organic nano particle is 200 ~ 500 nm.
3. the ice-covering-proof material of liquid filling cellular silicone according to claim 1, is characterized in that: the cellular silicone of silicon fluoride modification is joined by the base material being coated with cellular silicone in the encloses container being placed with silicon fluoride or immerse to be dissolved with in the solution of fluorine containing silane to carry out surface chemical modification and form.
4. the ice-covering-proof material of liquid filling cellular silicone according to claim 1, is characterized in that: described silicon fluoride is selected from one or more in trifluoroethyl Trimethoxy silane, trifluoroethyl Trimethoxy silane, hexafluoro butyl trimethoxy silane, hexafluoro butyl triethoxyl silane, five fluorine octyl group Trimethoxy silanes, five fluorine octyltri-ethoxysilane, perfluoro capryl Trimethoxy silane, perfluoro capryl triethoxy.
5. the ice-covering-proof material of liquid filling cellular silicone according to claim 1, is characterized in that: described inorganic silicon raw material is water glass, and organosilicon materials is selected from one or more in methyl silicate, tetraethoxy, positive isopropyl silicate.
6. the ice-covering-proof material of liquid filling cellular silicone according to claim 1, is characterized in that: described catalyst solution is aqueous acid, and described acid is selected from one or more in hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, formic acid, aqueous acetic acid.
7. the ice-covering-proof material of liquid filling cellular silicone according to claim 6, is characterized in that: described catalyst solution concentration range is 0.01 ~ 1mol/L; The volume ratio of catalyst solution and mixing solutions is 1:10 ~ 1:100.
8. the ice-covering-proof material of liquid filling cellular silicone according to claim 1, is characterized in that: described organic nano particle is selected from one or more in polystyrene, polymethylmethacrylate, polyacrylonitrile, polylactide, poly(lactic acid), nano-cellulose.
9. the ice-covering-proof material of liquid filling cellular silicone according to claim 1, is characterized in that: the mass ratio of described organic nano particle and inorganic silicon or organosilicon materials is 1:1 ~ 1:4.
10. the ice-covering-proof material of liquid filling cellular silicone according to claim 1, is characterized in that: the method for described removal organic nano particle comprises high temperature ablation or dissolution with solvents; The temperature province of described high temperature ablation is 300 ~ 800
oc, the ablation time is 0.5 ~ 20h; One or more in the solvent selected from chloroform used in described dissolution with solvents, methylene dichloride, tetracol phenixin, tetrahydrofuran (THF), dimethyl formamide, soak time is 2 ~ 24h.
The ice-covering-proof material of 11. liquid filling cellular silicone according to claim 1, is characterized in that: the solvent in described mixing solutions is selected from one or more in water, methyl alcohol, ethanol, propyl alcohol, Virahol, butanols, acetone.
The ice-covering-proof material of 12. liquid filling cellular silicone according to claim 1, is characterized in that: described base material is copper, iron, aluminium, titanium, glass or pottery.
13. 1 kinds of methods preparing the ice-covering-proof material of liquid filling cellular silicone described in any one of claim 1-12, is characterized in that, comprise following process:
(1) preparation of cellular silicone: organic nano particle is joined massfraction be 10% ~ 50% inorganic silicon or organic silicon solution in, after mixing, add catalyst solution, the mixing solutions formed directly is coated in substrate surface, and after solidification to be dried, high temperature ablation or dissolution with solvents are removed organic nano particle and obtained cellular silicone surface;
(2) cellular silicone surface chemical modification: the encloses container having the base material of cellular silicone to be placed on the surface that (1) step obtains to be placed with silicon fluoride or immerse and be dissolved with fluorine containing silane solution and carry out surface chemical modification;
(3) fluorine-containing liquid filling: adopt the method for spraying or immersion to be fixed in the cellular silicone of surface chemical modification by fluorine-containing liquid.
14. methods according to claim 13, is characterized in that: the time of described surface chemical modification is 2 ~ 48 h.
15. methods according to claim 13, is characterized in that: one or more in the solution of described fluorine containing silane in solvent selected from methanol, ethanol, acetone, benzene, chloroform; In described fluorine containing silane solution, the massfraction of fluorine containing silane is 1% ~ 20%.
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| CN101230224A (en) * | 2008-02-27 | 2008-07-30 | 孟中 | Fluorosilicone rubber nano composite alloy three-proof paint and production method thereof |
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