CN110294980A - A kind of preparation method of hydrophobic material - Google Patents
A kind of preparation method of hydrophobic material Download PDFInfo
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- CN110294980A CN110294980A CN201810247993.0A CN201810247993A CN110294980A CN 110294980 A CN110294980 A CN 110294980A CN 201810247993 A CN201810247993 A CN 201810247993A CN 110294980 A CN110294980 A CN 110294980A
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- Prior art keywords
- reaction
- temperature
- coating
- hydrophobic material
- fluorocarbon solvent
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Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D127/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers
- C09D127/02—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D127/12—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/65—Additives macromolecular
Abstract
There is superior hydrophobic property in order to solve general fluorine-containing macromolecule, Van der Waals force only between these fluoro containing polymers and substrate is very faint, cause fluoro containing polymers coating weaker with the adhesion strength between substrate, and the inadequate problem of hardness of coating, the present invention proposes a kind of preparation method of super hydrophobic material, the super hydrophobic material prepared using preparation method of the invention, using coating, it impregnates or the mode of vacuum coating is transferred to substrate surface, form super-hydrophobic coat, good hydrophobic performance can not only be played, also there is preferable coating hardness simultaneously.
Description
Technical field
The present invention relates to hydrophobic coating field technologies, are specifically related to a kind of preparation method of super hydrophobic material.
Background technique
Anti-pollution, anti-fingerprint film layer function be reduce body surface surface can (such as glass or metal watch energy), formed
A kind of film layer of superhydrophobic characteristic.Changing body surface can be there are two types of method, and one is physical rough surface to modify method: according to
Self-cleaning theory, surface texture is more coarse, can produce more excellent hydrophobic self-cleaning effect, but coarse surface can cause visible light
Significant divergence makes coating that non-transparent state be presented, and makes mechanicalness, and such as then, wear-resistant and other effects decline, the method protect in current
Shield glass industries are simultaneously not suitable for；Another method is added on the group to macromolecular chain of fluorine functional group, along with hydrogen on alkyl
Atom is replaced by fluorine atoms the increase of number, and surface can also decline therewith, and material surface can form minimum surface energy and highest
The material of water droplet feeler, the material of all plane surface structures and the contact angle of water do not exceed 120 °, therefore, general fluorine-containing
Macromolecule has superior hydrophobic property, and only the Van der Waals force between these fluoro containing polymers and substrate is very faint, causes to contain
Fluorine polymeric coating layer is weaker with the adhesion strength between substrate, and the hardness of coating is inadequate.
Summary of the invention
In view of this, the present invention proposes a kind of preparation method of super hydrophobic material, using preparation method system of the invention
Standby super hydrophobic material out, is transferred to substrate surface using coating, immersion or vacuum coating mode, forms super-hydrophobic painting
Layer can not only play good hydrophobic performance, while also have preferable coating hardness.
A kind of super hydrophobic material needs to weigh the raw material of following mass percent during configuration:
Modified perfluoropolyether is a: 13%~15%；
Each three parts: 24.3%~24.8% of fluorine carbon solution (I)；
Silane coupling agent is a: 1.2%~1.5%；
Fluorocarbon solvent (II) is a: 41%~42%；
Acyl fluorides dimer is a: 4.5%~4.8%；
Each two parts: 13%~15% of anhydrous methanol.
A kind of preparation method of super hydrophobic material comprising following steps:
Step1, it is molten successively to put into modified perfluoropolyether, fluorine carbon in a kettle for the ratio of raw material as described above
Agent (I) and silane coupling agent reaction, sets reaction temperature as 40 DEG C, the reaction time 2 hours, at the same control ambient humidity for 30 ±
5%, 20 ± 5 DEG C of temperature；
Anhydrous methanol in the reaction product of step Step1 and raw material ratio as described above is added to point by Step2
In liquid funnel, being stood after shaking up, the liquid in separatory funnel is divided into two layers, and supernatant liquid is unreacted silane coupling agent, under
Layer liquid is target product layer, and lower liquid is separated, and then rotates out extra fluorocarbon solvent using rotary evaporator
(1), revolving temperature is 40 DEG C, is rotated until products weight is no longer reduced, spare.
Step3, the product and fluorocarbon solvent (I) and acyl fluorides dimer that step Step2 processing is completed are according to raw material
Mass ratio successively puts into reaction kettle, sets reaction temperature as 40 DEG C, the reaction time 2 hours, while controlling ambient humidity is 30
± 5%, 20 ± 5 DEG C of temperature；
Step4, by step Step3 reaction product and anhydrous methanol, fluorocarbon solvent (I) according to raw material mass ratio
Reaction kettle is successively put into, reacts 30min, after the reaction was completed stratification, isolates supernatant liquid, lower liquid is that reaction produces
Object.
Step5 distills fluorine carbon solution (I) extra in the reaction product in Step4, and revolving temperature is set as 30
DEG C, it is threaded to until weight no longer mitigates.
Reaction product in step Step5 is diluted to prescribed concentration using fluorocarbon solvent (II), can be obtained by Step6
Hydrophobic film coating liuqid of the invention.
Further, the storage concentration of water delivery coating liquid of the invention is 20%, and temperature is 20 DEG C, and humidity 5% uses
When concentration be 0.01%~0.03%.
Further, silane coupling agent is vinyl silanes, amino silane, epoxy radicals silicone hydride, hydrosulphonyl silane and methyl-prop
One of alkene acyloxy silane.
The reaction principle of super hydrophobic material of the invention are as follows: perfluoropolyether containing methoxyl group is anti-with amino silicane coupling agent
It answers, amino and methoxyl group carry out substitution reaction, and the perfluoropolyether for being connected to amino silane, silane coupling agent reactivity are obtained after reaction
By force, can with most surfaces hydroxyl, carboxyl isoreactivity group substrate in conjunction with, thus substrate surface formed one layer of villiform
Monolayer, due to the physical characteristic of its microstructure and perfluoropolyether segment itself, so that it is good to have substrate surface
Smooth and hydrophobic oleophobic performance, for hydrophobic angle up to 119 °, and due to being monolayer, hardness keeps one with substrate substantially
It causes, using effect is excellent on Coating Materials.
The super hydrophobic material prepared using method of the invention can be true using coating, immersion or plasmaassisted
Super hydrophobic material is transferred to substrate surface by empty evaporation coating mode, to increase the hydrophobic performance of substrate surface, promotes base
The smoothness on material surface, and guarantee the hardness of coating.
Detailed description of the invention
Fig. 1 is the schematic arrangement of modification perfluoropolyether of the invention.
Fig. 2 is the schematic arrangement of two kinds of fluorine carbon solutions.
Fig. 3 is the schematic arrangement of amino silane.
The present invention that the following detailed description will be further explained with reference to the above drawings.
Specific embodiment
Case 1 is embodied:
One of this implementation 1 super hydrophobic material needs to weigh the original of following mass percent during configuration
Material:
Modified perfluoropolyether is a: 14%；
Each three parts: 24.6% of fluorine carbon solution (I)；
Silane coupling agent is a: 1.3%；
Fluorocarbon solvent (II) is a: 41.5%；
Acyl fluorides dimer is a: 4.6%；
Each two parts: 14% of anhydrous methanol.
Case 2 is embodied:
One of this implementation 2 super hydrophobic material needs to weigh the original of following mass percent during configuration
Material:
Modified perfluoropolyether is a: 13.5%；
Each three parts: 24.4% of fluorine carbon solution (I)；
Silane coupling agent is a: 1.4%；
Fluorocarbon solvent (II) is a: 41.2%；
Acyl fluorides dimer is a: 4.6%；
Each two parts: 14.9% of anhydrous methanol.
Case 3 is embodied:
One of this implementation 3 super hydrophobic material needs to weigh the original of following mass percent during configuration
Material:
Modified perfluoropolyether is a: 14.5%；
Each three parts: 24.5% of fluorine carbon solution (I)；
Silane coupling agent is a: 1.35%；
Fluorocarbon solvent (II) is a: 41.8%；
Acyl fluorides dimer is a: 4.7%；
Each two parts: 13.15% of anhydrous methanol.
The preparation method of super hydrophobic material in specific embodiment 1~3, follows the steps below preparation:
Step1, it is molten successively to put into modified perfluoropolyether, fluorine carbon in a kettle for the ratio of raw material as described above
Agent (I) and silane coupling agent reaction, sets reaction temperature as 40 DEG C, the reaction time 2 hours, at the same control ambient humidity for 30 ±
5%, 20 ± 5 DEG C of temperature；
Anhydrous methanol in the reaction product of step Step1 and raw material ratio as described above is added to point by Step2
In liquid funnel, being stood after shaking up, the liquid in separatory funnel is divided into two layers, and supernatant liquid is unreacted silane coupling agent, under
Layer liquid is target product layer, and lower liquid is separated, and then rotates out extra fluorocarbon solvent using rotary evaporator
(1), revolving temperature is 40 DEG C, is rotated until products weight is no longer reduced, spare.
Step3, the product and fluorocarbon solvent (I) and acyl fluorides dimer that step Step2 processing is completed are according to raw material
Mass ratio successively puts into reaction kettle, sets reaction temperature as 40 DEG C, the reaction time 2 hours, while controlling ambient humidity is 30
± 5%, 20 ± 5 DEG C of temperature；
Step4, by step Step3 reaction product and anhydrous methanol, fluorocarbon solvent (I) according to raw material mass ratio
Reaction kettle is successively put into, reacts 30min, after the reaction was completed stratification, isolates supernatant liquid, lower liquid is that reaction produces
Object.
Step5 distills fluorine carbon solution (I) extra in the reaction product in Step4, and revolving temperature is set as 30
DEG C, it is threaded to until weight no longer mitigates.
Reaction product in step Step5 is diluted to prescribed concentration using fluorocarbon solvent (II), can be obtained by Step6
Hydrophobic film coating liuqid of the invention.
Wherein, silane coupling agent as described above uses amino silane.
Further, the storage concentration of super hydrophobic material of the invention is 20%, and temperature is 20 DEG C, and humidity 5% makes
With when concentration be 0.01%~0.03%.
The super hydrophobic material that the acquisition in case 1~3 is embodied can be assisted being evaporated in vacuo with using plasma
Super hydrophobic material is transferred to glass substrate surface by plated film mode, and specific implementation case 1~3 is shown in test result is as follows:
1. steel wool wear-resisting property detects: 1cm × 1cm bistrique；Load 1000g；Stroke 4.5cm；3000 wear-resisting tests
100 ° of hydrophobic angle > afterwards
2. erasing rubber wear-resisting property detects: diameter 6.5mm loads 1000g, stroke 2cm；It is hydrophobic after 3000 wear-resisting tests
100 ° of angle >
It can be seen that the super hydrophobic material prepared using method of the invention, using plasma auxiliary is evaporated in vacuo
Hydrophobic film coating liuqid is transferred to glass substrate surface by plated film mode, can increase the hydrophobic performance of glass surface, promotes glass table
The smoothness in face, and guarantee the hardness of coating.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
Limitations on the scope of the patent of the present invention therefore cannot be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to guarantor of the invention
Protect range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (5)
1. a kind of preparation method of super hydrophobic material comprising following steps:
Step1, the raw material for weighing following mass percent are spare:
Modified perfluoropolyether is a: 13%~15%;
Each three parts: 24.3%~24.8% of fluorine carbon solution (I);
Silane coupling agent is a: 1.2%~1.5%；
Fluorocarbon solvent (II) is a: 41%~42%；
Acyl fluorides dimer is a: 4.5%~4.8%;
Each two parts: 13%~15% of anhydrous methanol；
Step2, the ratio of raw material successively puts into modified perfluoropolyether, fluorocarbon solvent in a kettle as described above
(I) reacted with silane coupling agent, set reaction temperature as 40 DEG C, the reaction time 2 hours, at the same control ambient humidity for 30 ±
5%, 20 ± 5 DEG C of temperature；
Anhydrous methanol in the reaction product of step Step2 and raw material ratio as described above is added to liquid separation leakage by Step3
It in bucket, is stood after shaking up, the liquid in separatory funnel is divided into two layers, and supernatant liquid is unreacted silane coupling agent, subnatant
Body is target product layer, and lower liquid is separated, and then rotates out extra fluorocarbon solvent (1) using rotary evaporator,
Rotating temperature is 40 DEG C, is rotated until products weight is no longer reduced, spare;
Step Step3 is handled the product completed and fluorocarbon solvent (I) and acyl fluorides dimer according to the quality of raw material by Step4
Than successively putting into reaction kettle, reaction temperature is set as 40 DEG C, the reaction time 2 hours, while controlling ambient humidity is 30 ± 5%,
20 ± 5 DEG C of temperature；
Step5, by step Step4 reaction product and anhydrous methanol, fluorocarbon solvent (I) according to raw material mass ratio successively
Reaction kettle is put into, reacts 30min, stratification, isolates supernatant liquid after the reaction was completed, and lower liquid is reaction product;
Step6 distills fluorine carbon solution (I) extra in the reaction product in Step5, and revolving temperature is set as 30 DEG C,
It is threaded to until weight no longer mitigates;
Reaction product in step Step6 is diluted to prescribed concentration using fluorocarbon solvent (II), this hair can be obtained by Step7
Bright hydrophobic film coating liuqid.
2. the preparation method of super hydrophobic material as described in claim 1, it is characterised in that: the hydrophobic plating in step Step7
The storage concentration of film liquid is 20%, and temperature is 20 DEG C, humidity 5%, and the concentration of the use of time is 0.01%~0.03%.
3. the preparation method of super hydrophobic material as described in claim 1, it is characterised in that: silane coupling agent is vinyl silicon
One of alkane, amino silane, epoxy radicals silicone hydride, hydrosulphonyl silane and methacryloxypropyl silane.
4. the super hydrophobic material being prepared using method of claim 1.
5. the super hydrophobic material being prepared using method of claim 1 is true using coating, immersion or plasmaassisted
Empty evaporation coating mode is transferred to the application of substrate surface.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810247993.0A CN110294980A (en) | 2018-03-23 | 2018-03-23 | A kind of preparation method of hydrophobic material |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810247993.0A CN110294980A (en) | 2018-03-23 | 2018-03-23 | A kind of preparation method of hydrophobic material |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103865390A (en) * | 2012-12-18 | 2014-06-18 | 锜玮科技(深圳)有限公司 | Hydrophobic film-coating liquid and production process of anti-pollution anti-fingerprint film-coated layer prepared therefrom |
| US20150004861A1 (en) * | 2013-06-30 | 2015-01-01 | Xerox Corporation | Grafted polymers as oleophobic or hydrophobic coatings |
| CN105524552A (en) * | 2016-01-18 | 2016-04-27 | 矽时代材料科技股份有限公司 | High performance organic silicon-fluorine nano-paint and use of same |
| CN106883405A (en) * | 2015-12-15 | 2017-06-23 | 比亚迪股份有限公司 | A kind of silane-modified fluoropolymer and preparation method thereof and anti-fingerprint coating |
-
2018
- 2018-03-23 CN CN201810247993.0A patent/CN110294980A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103865390A (en) * | 2012-12-18 | 2014-06-18 | 锜玮科技(深圳)有限公司 | Hydrophobic film-coating liquid and production process of anti-pollution anti-fingerprint film-coated layer prepared therefrom |
| US20150004861A1 (en) * | 2013-06-30 | 2015-01-01 | Xerox Corporation | Grafted polymers as oleophobic or hydrophobic coatings |
| CN106883405A (en) * | 2015-12-15 | 2017-06-23 | 比亚迪股份有限公司 | A kind of silane-modified fluoropolymer and preparation method thereof and anti-fingerprint coating |
| CN105524552A (en) * | 2016-01-18 | 2016-04-27 | 矽时代材料科技股份有限公司 | High performance organic silicon-fluorine nano-paint and use of same |
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Application publication date: 20191001 |