CN103788853B - The preparation method of the super two open coat of a kind of urethane/molybdenumdisulphide - Google Patents
The preparation method of the super two open coat of a kind of urethane/molybdenumdisulphide Download PDFInfo
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Abstract
The present invention relates to super two thin field of material technology, more particularly, relate to the preparation method of super-hydrophobic, the super oleophobic films coating of a kind of urethane/molybdenumdisulphide.First the present invention prepares urethane/molybdenumdisulphide composite micro/nano grade uneven surface by spraying method, and the contact angle of coatingsurface and water is greater than 150 °, then passes through 1H, 1H, 2H, 2H-perfluor octyloxy trichlorosilane finish coat, the coatingsurface obtained has ultra-amphosphobic.This ultra-amphosphobic surface all has repellency to water, glycerine, ethylene glycol, rapeseed oil, n-Hexadecane etc.Wherein be greater than 160 ° with the contact angle of water, roll angle is less than 3 °.All be greater than 150 ° with the contact angle of n-Hexadecane, vegetable seed wet goods liquid, roll angle is all less than 10 °.Super two open coat that the method is prepared has higher stability, can be sprayed on the material of unlike material, and technique is simple, is easy to big area and prepares super-double-hydrophobic surface, be easy to realize industrialization manufacture.
Description
Technical field
The present invention relates to super two thin field of material technology, more particularly, relate to the preparation method of super-hydrophobic, the super oleophobic films coating of a kind of urethane/molybdenumdisulphide.
Background technology
There is a large amount of super hydrophobic surfaces in occurring in nature, refers to contact angle and be greater than 150 °, the roll angle uneven surface that is less than 10 °; Researchist is by the bionics fiber to leaf surface of plant superhydrophobic characteristic, proposing the emphasis preparing super hydrophobic surface is effectively construct coarse surface tissue and carry out surface chemical modification to reduce surface energy, and achieves some impressive progresses in the preparation method of super hydrophobic surface, formation mechenism and functionalization research etc.; But super hydrophobic surface in use inevitably contacts some oleaginous materials, these material surface tension force are lower, are easy to infiltrate surface, and are difficult to removing, and ultra-hydrophobicity very easily affects by it; Such as, drip n-Hexadecane at lotus leaf surface, n-Hexadecane will be sprawled rapidly, and its contact angle is 0 °, will be lost the performance of its super-hydrophobic automatic cleaning by the lotus leaf that n-Hexadecane infiltrates; For the problem of super hydrophobic surface oil rub resistance ability, the concept that Jiang Lei etc. first proposed " super two thin ", the contact angle referring to water and oil is all greater than the surface of 150 °, that is have the surface of super-hydrophobic and super oleophobic, the drop of different surfaces tension force can roll arbitrarily on surface and can not infiltrate surface simultaneously; Relative to the super hydrophobic surface of simple function, super-double-hydrophobic surface has boundless application prospect in industrial and agricultural production He in daily life, such as, super oleophobic material can be applied on the shell of boats and ships, fuel reserve tank, can realize anticorrosion, reduce the effects such as friction, preventing pollution; Transport for petroleum pipe line and can prevent oil sticking duct wall, thus the loss reduced in transportation and energy expenditure, and the blockage problem of petroleum pipe line can be reduced; Can also apply on the textile, make the clothes etc. of waterproof and oil rub resistance.
The wide application prospect had due to super-double-hydrophobic surface and researching value, people utilize various method and access to prepare this surface; In recent years, researchist, by special surface-texturing and modifying method, on silicon substrate, metallic surface, fabric, fluorinated polymer and nano particle, has prepared a series of surface with ultra-amphosphobic energy; The theoretical investigation of these results of study to super oleophobic surface has very important meaning and is expected to move towards practical application; Even so, but some problems are had still to need solution, as strict preparation condition, loaded down with trivial details step, expensive material and poor stability and wearing quality; Therefore, invent a kind of simple and be easy to the technology of industrialization, super two thin surface can be constructed be very important on any matrix.
Summary of the invention
The invention provides the preparation method of the super two open coat of a kind of urethane/molybdenumdisulphide, for realizing the hydrophobic of the substrate surface such as metal, glass and oleophobic performance, the method preparation flow is simple, two thin performance is strong, preparation cost is low, and it is convenient to implement, and can carry out large-scale promotion; The contact angle of super two open coat of the present invention and water and oil is all greater than 150 °, and has the characteristic of low adhesion, and super two open coat of the present invention can be applicable in pipeline transportation, navigation and daily life.
The invention provides the preparation method of the super two open coat of a kind of urethane/molybdenumdisulphide, its technique is:
(1) take the urethane resin of certain mass, use one or both solvent cuts in ethyl acetate, acetone, the volume of solvent and urethane resin and mass ratio are 10-25:1, and magnetic agitation is to even.
(2) take a certain proportion of molybdenumdisulphide, be diluted in polyurethane resin solution, after mixing, stand-by.
(3) under a nitrogen, on the base material to be coated after the pre-treatment by material spraying, insert air dry oven solidification treatment after seasoning, furnace cooling, obtain super-hydrophobic coat.
(4) super-hydrophobic coat that step (3) obtains is put into vacuum vessel, putting into subsequently to drip has 1H, the weighing bottle of 1H, 2H, 2H-perfluor octyloxy trichlorosilane, and sealing, vacuumizes, airtight maintenance 5-20min, venting, takes out sample.
(5) super two open coat is obtained after sample drying step (4) obtained.
Described urethane and the mass ratio of molybdenumdisulphide are 0.5-2:1.
Described mixing refers to magnetic agitation 2h, sonic oscillation 20-60min.
Described solvent is one or both in ethyl acetate, acetone, and the volume ratio of both consumptions is acetone 0%-50%, ethyl acetate 50%-100%.
The pressure of described nitrogen is 0.2-0.5Mpa, and by material spraying after the pre-treatment base material to be coated, after seasoning 20min, insert air dry oven 80-120 DEG C solidification treatment 1-2h, furnace cooling, obtains super-hydrophobic coat.
Described 1H, 1H, 2H, 2H-perfluor octyloxy trichlorosilane modifies urethane/molybdenumdisulphide compound coating by vapour deposition, reduces surface energy, in conjunction with spraying gained micro-/ nano grade coarse structure, makes coating have ultra-amphosphobic energy; Conventional glue head dropper is adopted to drip 1H, 1H, 2H, 2H-perfluor octyloxy trichlorosilane to weighing bottle instillation 3-5.
The described vacuum tightness vacuumized is 0.09Mpa.
This ultra-amphosphobic surface all has repellency to water, glycerine, ethylene glycol, rapeseed oil, n-Hexadecane etc., and be wherein greater than 160 ° with the contact angle of water, roll angle is less than 3 °; All be greater than 150 ° with the contact angle of n-Hexadecane, vegetable seed wet goods liquid, roll angle is all less than 10 °.
Accompanying drawing explanation
Fig. 1 is the contact angle photo of super two open coat and water.
Fig. 2 is the contact angle photo of super two open coat and n-Hexadecane.
Fig. 3 is the photo of prepared super two open coat on slide glass.
Fig. 4 is the SEM figure of super two open coat.
Embodiment
Embodiment 1:
The first step, takes the urethane resin of 2.0g, and use the ethyl acetate solution dilution of 20mL, magnetic agitation is uniformly dissolved; Take 1.5g molybdenumdisulphide again, add in polyurethane resin solution, magnetic agitation 2h, sonic oscillation 20min.
Second step, selects the 45# bloom of 500# abrasive paper for metallograph polishing specification 20mm × 10mm × 10mm, and after polishing smooth, insert ultrasonic in acetone soln cleaning, taking-up is dried.
3rd step, material spraying step one obtained under 0.2Mpa nitrogen is on the base material that step 2 is processed, and thickness 20 μm, after natural air drying 20min, inserts 80 DEG C of solidification 2h in air dry oven.
4th step, storage period after step 3 cooling is put into vacuum vessel more than the sample of 12h, will drip and have 1H, 1H, 2H, the weighing bottle of 2H-perfluor octyloxy trichlorosilane is uncovered to be put into wherein simultaneously, and sealing, vacuumizes, being evacuated to vacuum values is 0.09Mpa, airtight, after vapour deposition 5min, sample is taken out in venting.
5th step, puts into air dry oven 100 DEG C of dry 1h by the sample obtained, after furnace cooling, obtain super two open coat.
Embodiment 2:
The first step, takes the urethane resin of 2.0g, and use ethyl acetate and the dilution of 15mL acetone mixed solvent of 15mL, magnetic agitation is uniformly dissolved; Take 2.0g molybdenumdisulphide again, add in polyurethane resin solution, magnetic agitation 2h, sonic oscillation 30min.
Second step, selects the tinplate sheet of 500# abrasive paper for metallograph polishing specification 120mm × 50mm × 1mm, and after polishing smooth, insert ultrasonic in acetone soln cleaning, taking-up is dried.
3rd step, material spraying step one obtained under 0.3Mpa nitrogen is on the base material that step 2 is processed, and thickness 30 μm, after natural air drying 20min, inserts 100 DEG C of solidification 1.5h in air dry oven.
4th step, storage period after step 3 cooling is put into vacuum vessel more than the sample of 12h, will drip and have 1H, 1H, 2H, the weighing bottle of 2H-perfluor octyloxy trichlorosilane is uncovered to be put into wherein simultaneously, and sealing, vacuumizes, being evacuated to vacuum values is 0.09Mpa, airtight, after vapour deposition 10min, sample is taken out in venting.
5th step, puts into air dry oven 100 DEG C of dry 1h by the sample obtained, after furnace cooling, obtain super two open coat.
Embodiment 3:
The first step, takes the urethane resin of 2.0g, and use ethyl acetate and the dilution of 15mL acetone mixed solvent of 25mL, magnetic agitation is uniformly dissolved; Take 2.5g molybdenumdisulphide again, add in polyurethane resin solution, magnetic agitation 2h, sonic oscillation 40min.
Second step, selects specification to be the slide glass of 76.4mm × 25mm × 1mm, by the cotton balls wiping surface of glass slide being moistened with acetone soln, wipes clean and dries.
3rd step, material spraying step one obtained under 0.4Mpa nitrogen is on the base material that step 2 is processed, and thickness 40 μm, after natural air drying 20min, inserts 120 DEG C of solidification 1h in air dry oven.
4th step, storage period after step 3 cooling is put into vacuum vessel more than the sample of 12h, will drip and have 1H, 1H, 2H, the weighing bottle of 2H-perfluor octyloxy trichlorosilane is uncovered to be put into wherein simultaneously, and sealing, vacuumizes, being evacuated to vacuum values is 0.09Mpa, airtight, after vapour deposition 15min, sample is taken out in venting.
5th step, puts into air dry oven 100 DEG C of dry 1h by the sample obtained, after furnace cooling, obtain super two open coat.
Embodiment 4:
The first step, takes the urethane resin of 1.5g, and use ethyl acetate and the dilution of 15mL acetone mixed solvent of 22.5mL, magnetic agitation is uniformly dissolved; Take 3.0g molybdenumdisulphide again, add in polyurethane resin solution, magnetic agitation 2h, sonic oscillation 60min.
Second step, selects specification to be on the stainless (steel) wire of 20mm × 20mm × 0.2mm, and insert ultrasonic in acetone soln cleaning, taking-up is dried.
3rd step, material spraying step one obtained under 0.5Mpa nitrogen is on the base material that step 2 is processed, and thickness 50 μm, after natural air drying 20min, inserts 120 DEG C of solidification 1h in air dry oven.
4th step, storage period after step 3 cooling is put into vacuum vessel more than the sample of 12h, will drip and have 1H, 1H, 2H, the weighing bottle of 2H-perfluor octyloxy trichlorosilane is uncovered to be put into wherein simultaneously, and sealing, vacuumizes, being evacuated to vacuum values is 0.09Mpa, airtight, after vapour deposition 20min, sample is taken out in venting.
5th step, puts into air dry oven 100 DEG C of dry 1h by the sample obtained, after furnace cooling, obtain super two open coat.
In Fig. 1 and Fig. 2, super-double-hydrophobic surface material to water and n-Hexadecane contact angle be all greater than 150 °, be respectively 167.5 °, 155.5 °.
Can to find out in Fig. 3 under room temperature that from left to right, water, n-Hexadecane, ethylene glycol all present spherical state at super two open coat, can see to have the microtexture that micro-/ nano grade is coarse by surface uniform prepared by the two open coat of excess of export in Fig. 4 SEM figure.
Claims (7)
1. a preparation method for the super two open coat of urethane/molybdenumdisulphide, is characterized in that comprising the steps:
(1) take the urethane resin of certain mass, use one or both solvent cuts in ethyl acetate, acetone, the volume of solvent and urethane resin and mass ratio are 10-25mL:1g, and magnetic agitation is to even;
(2) take a certain proportion of molybdenumdisulphide, be diluted in polyurethane resin solution, after mixing, stand-by;
(3) under a nitrogen, on the base material to be coated after the pre-treatment by material spraying, insert air dry oven solidification treatment after seasoning, furnace cooling, obtain super-hydrophobic coat;
(4) super-hydrophobic coat that step (3) obtains is put into vacuum vessel, putting into subsequently to drip has 1H, the weighing bottle of 1H, 2H, 2H-perfluor octyloxy trichlorosilane, and sealing, vacuumizes, airtight maintenance 5-20min, venting, takes out sample;
(5) super two open coat is obtained after sample drying step (4) obtained.
2. the preparation method of the super two open coat of a kind of urethane/molybdenumdisulphide as claimed in claim 1, is characterized in that: described urethane and the mass ratio of molybdenumdisulphide are 0.5-2:1.
3. the preparation method of the super two open coat of a kind of urethane/molybdenumdisulphide as claimed in claim 1, is characterized in that: described mixing refers to magnetic agitation 2h, sonic oscillation 20-60min.
4. the preparation method of the super two open coat of a kind of urethane/molybdenumdisulphide as claimed in claim 1, it is characterized in that: described solvent is one or both in ethyl acetate, acetone, the volume ratio of both consumptions is acetone 0%-50%, ethyl acetate 50%-100%.
5. the preparation method of the super two open coat of a kind of urethane/molybdenumdisulphide as claimed in claim 1, it is characterized in that: the pressure of described nitrogen is 0.2-0.5MPa, by on material spraying after the pre-treatment base material to be coated, after seasoning 20min, insert air dry oven 80-120 DEG C solidification treatment 1-2h, furnace cooling, obtains super-hydrophobic coat.
6. the preparation method of the super two open coat of a kind of urethane/molybdenumdisulphide as claimed in claim 1, it is characterized in that: described 1H, 1H, 2H, 2H-perfluor octyloxy trichlorosilane modifies urethane/molybdenumdisulphide compound coating by vapour deposition, reduce surface energy, in conjunction with spraying gained micro-/ nano grade coarse structure, make coating have ultra-amphosphobic energy; Conventional glue head dropper is adopted to drip 1H, 1H, 2H, 2H-perfluor octyloxy trichlorosilane to weighing bottle instillation 3-5.
7. the preparation method of the super two open coat of a kind of urethane/molybdenumdisulphide as claimed in claim 1, is characterized in that: described in the vacuum tightness that vacuumizes be 0.09MPa.
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| CN106049050A (en) * | 2016-06-27 | 2016-10-26 | 安庆石油化工总厂联盟化工厂 | Woven bag coating method |
| CN109173747B (en) * | 2018-09-21 | 2020-12-04 | 苏州大学 | Multi-walled carbon nanotube self-repairing film, preparation method thereof and application thereof in treating oil-containing wastewater |
| CN109807044A (en) * | 2019-04-12 | 2019-05-28 | 东北农业大学 | Pneumatic equipment bladess coat molybdenum sulfide nanometer ice-phobic coating technical method |
| WO2022011566A1 (en) * | 2020-07-14 | 2022-01-20 | 重庆康佳光电技术研究院有限公司 | Transfer substrate and manufacturing method therefor, and chip transfer method |
| CN114985236B (en) * | 2022-07-14 | 2023-09-19 | 国网福建省电力有限公司电力科学研究院 | Preparation method of super-hydrophobic antifouling coating on surface of glass insulator |
| CN116376431A (en) * | 2023-03-28 | 2023-07-04 | 暨南大学 | Self-repairing super-hydrophobic protective packaging composite coating based on two-dimensional molybdenum sulfide and preparation method and application thereof |
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| CN1221769A (en) * | 1997-12-30 | 1999-07-07 | 中国科学院兰州化学物理研究所 | Polyurethane normal temp. solidified anticorrosion lubricating paint |
| WO2006044653A1 (en) * | 2004-10-14 | 2006-04-27 | Akzo Nobel Coatings International B.V. | Iron carbonyl containing coating composition |
| CN1865370A (en) * | 2006-06-13 | 2006-11-22 | 中北大学 | Wax deposition resistant coating for oil pipeline |
| CN102453428A (en) * | 2010-10-29 | 2012-05-16 | 中国科学院兰州化学物理研究所 | Room-temperature solidified super-oleophobic polyurethane coating |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1221769A (en) * | 1997-12-30 | 1999-07-07 | 中国科学院兰州化学物理研究所 | Polyurethane normal temp. solidified anticorrosion lubricating paint |
| WO2006044653A1 (en) * | 2004-10-14 | 2006-04-27 | Akzo Nobel Coatings International B.V. | Iron carbonyl containing coating composition |
| CN1865370A (en) * | 2006-06-13 | 2006-11-22 | 中北大学 | Wax deposition resistant coating for oil pipeline |
| CN102453428A (en) * | 2010-10-29 | 2012-05-16 | 中国科学院兰州化学物理研究所 | Room-temperature solidified super-oleophobic polyurethane coating |
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Effective date of registration: 20200630 Address after: 222000 Economic Development Zone of Guanyun County, Lianyungang City, Jiangsu Province Patentee after: LIANYUNGANG ZEYANG DECORATIVE MATERIALS Co.,Ltd. Address before: Zhenjiang City, Jiangsu Province, 212013 Jingkou District Road No. 301 Patentee before: JIANGSU University |