CN104262663A - Preparation method of poly(phenol-amine) superhydrophobic particulates - Google Patents
Preparation method of poly(phenol-amine) superhydrophobic particulates Download PDFInfo
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- CN104262663A CN104262663A CN201410456954.3A CN201410456954A CN104262663A CN 104262663 A CN104262663 A CN 104262663A CN 201410456954 A CN201410456954 A CN 201410456954A CN 104262663 A CN104262663 A CN 104262663A
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Abstract
The invention discloses a preparation method of poly(phenol-amine) superhydrophobic particulates. The preparation method of the poly(phenol-amine) superhydrophobic particulates comprises the following steps: firstly adding a micro-nano material into a solution of polyphenol and polyamine, reacting for a period of time, and separating; and then dispersing the poly(phenol-amine) modified micro-nano material in a low surface energy matter solution for treatment, so that the superhydrophobic particulates are obtained. The preparation method of the poly(phenol-amine) superhydrophobic particulates is simple in process, easy to operate, controllable in technology, mild in conditions, good in repeatability, low in cost and convenient for popularization and application, the obtained poly(phenol-amine) superhydrophobic particulates have good superhydrophobic performance, can be applied to various materials and have a broad application range.
Description
Technical field
The present invention relates to material surface to modify and organic-inorganic Material cladding field, being specifically related to utilize the amine-modified micro Nano material of poly-phenol also by modifying the method that low-surface energy substance prepares super hydrophobic material further.
Background technology
Wettability is one of critical nature of solid surface, usually characterizes the infiltration degree of liquid versus solid with contact angle (contact angle, CA).The wettability of solid surface to fundamental research and practical application all extremely important, in recent years, super hydrophobic surface receives the extensive concern of people as a kind of very special phenomenon.Super hydrophobic surface generally refers to the surface with the contact angle > 150 ° of water, there is antifouling, waterproof, snow defence, anti-pollution, antiblocking, anti-oxidant, protection against corrosion, automatically cleaning and reducing noise and drag and prevent the important feature such as conduction of current, can be widely used in scientific research and the numerous areas such as production, life.
Find after deliberation, make preparation material there is ultra-hydrophobicity must meet two key conditions: one is that material surface has enough roughness, especially has micro-nano double scales structure; Two are surfacings is hydrophobic material, and namely surfacing is low-surface energy substance.For realizing this 2 point, usual method is in uneven surface modification low-surface energy substance or at low-surface energy substance surface construction coarse structure.At present, the method preparing super hydrophobic surface mainly contains following several method: template, etching method, chemical Vapor deposition process, electrochemical method, colloidal sol-gel method, electrostatic spinning technique etc.But just current present Research, also there is series of problems needs to solve: (1) current preparation technology is only limitted to the preparation of small area super hydrophobic surface, and the preparation of big area super hydrophobic surface still has difficulties; (2) preparation method of some super hydrophobic surfaces requires very high to substrate itself, and preparation condition is harsh, and manufacturing cost is high; (3) preparation method of some super hydrophobic surfaces needs the plant and instrument of complex precise, somewhat expensive and the cycle longer.
Inspire by adhesion protein, the people such as Lee are with simultaneously containing sticking component in the Dopamine HCL simulation adhesion protein of pyrocatechol and amido, research finds that Dopamine HCL can gather Dopamine HCL film by mode, the surperficial formation of organic materials inorganic in the overwhelming majority of oxidation auto-polymerization, and its result of study was published on Science in 2007.Because poly-Dopamine HCL has, Film build range is wide, experiment condition simple, at inorganic material surface grafting organic materials, in advantages such as organic materials surface deposition inorganic materials, subsequently, be widely used in surface modification, anticorrosion anti-corruption, detect the numerous areas such as sensing, antibiotic and sterilizing, catalyzed degradation, extracting and separating, medicine and transplanting.The present invention utilizes polyphenol and polyamines polymerization to modify micro Nano material, and prepares super-hydrophobic particulate by low-surface energy substance modification.
Summary of the invention
The object of the invention is to the deficiency overcoming prior art existence, and the preparation method of the super-hydrophobic particulate of a kind of poly-phenol amine is provided, this preparation method's process is simple, easy to operate, technique is controlled, mild condition, reproducible, with low cost, be convenient to promote the use of, obtained super-hydrophobic particulate has good ultra-hydrophobicity, and can be applied in various material, be with a wide range of applications.
For realizing object of the present invention, provide following technical scheme:
A preparation method for the super-hydrophobic particulate of poly-phenol amine, is characterized in that following steps:
(1) micro Nano material is joined in the solution of polyphenol and polyamines, be separated after reaction certain hour, the micro Nano material that obtained poly-phenol is amine-modified;
(2) step (1) gained is gathered the solution that the amine-modified micro Nano material of phenol is scattered in low-surface energy substance, be separated after reaction certain hour, the particulate with ultra-hydrophobicity can be obtained.
Further, in described step, micro Nano material is at least one in silicon-dioxide, titanium dioxide, aluminum oxide, zinc oxide, polymer microballoon, carbon nanotube.
Further, in described step, polyphenol is at least one in pyrocatechol, Resorcinol or Resorcinol.
Further, in described step, polyamines is phenylenediamine or structural formula is NH
2(CH
2) nNH
2aliphatic amide, n represents the integer of 6 to 30, at least one.
Further, in described step, the mass ratio of micro Nano material and polyphenol is 1: 0.02 ~ 1.
Further, in described step, the molar mass ratio of polyphenol and diamines is 1: 0.9 ~ 1.1.
Further, the micro Nano material that in described step, poly-phenol is amine-modified and the mass ratio of low-surface energy substance are 1: 0.1 ~ 1.1.
Further, in described step, low-surface energy substance is one in long-chain fat amine, long-chain fat mercaptan, perfluoroalkyl amine or mixture, and wherein long-chain fat amine structure formula is CH
3(CH
2)
nnH
2, n represents the integer of 9 to 30, and long-chain fat mercaptan structural formula is CH
3(CH
2)
nsH, n represent the integer of 9 to 30, and perfluoroalkyl amine structure formula is CF
3(CF
2)
n(CH
2)
mnH
2, n represents the integer of 5 to 10, and m represents the integer of 1 to 2.
The method tool that preparation of the present invention gathers the super-hydrophobic particulate of phenol amine has the following advantages:
(1) preparation method is easy to operate, technique is controlled, mild condition;
(2) prepare the with low cost of super-hydrophobic particulate, be convenient to promote the use of;
(3) obtained super-hydrophobic particulate has good ultra-hydrophobicity;
(4) obtained super-hydrophobic particulate can be applied in various material, is with a wide range of applications;
(5) the method preparation process is simpler and easy, and can be used for a large amount of generation fast, preparation cycle is short.
Accompanying drawing explanation
Fig. 1 is the aspect graph of the globule of the present invention at super-hydrophobic particle surface.
Embodiment
Below in conjunction with the drawings and specific embodiments, the invention will be further described.Following examples are intended to the present invention instead of limitation of the invention further are described.
Embodiment 1:
Reference (functional materials, 2008,8 (39), 1402) prepares particle diameter about 1 μm and the polystyrene microsphere that is evenly distributed (PS microballoon).Obtained PS microballoon being added to concentration is, in the pyrocatechol of 0.03mol/L and the aqueous solution of hexanediamine, under magnetic stirrer, react 24h, then centrifugal; Ultrasonic dispersion is utilized by obtained PCA@PS particulate to be dispersed in 0.1mol/L stearylamine ethanolic soln 1 hour, then vacuum-drying at 40 DEG C, i.e. the obtained poly-phenol amine particulate with ultra-hydrophobicity.
Embodiment 2:
By the silicon-dioxide (SiO of particle diameter 5-10 μm
2) to add concentration to be, in the pyrocatechol of 0.1mol/L and the ethanolic soln of hexanediamine, under magnetic stirrer, react 36h to microballoon, then centrifugal; By obtained PCA@SiO
2particulate utilizes ultrasonic dispersion to be dispersed in the Dodecyl Mercaptan ethanolic soln of 0.1mol/L 0.5 hour, then vacuum-drying at 40 DEG C, i.e. the obtained poly-phenol amine particulate with ultra-hydrophobicity.
Embodiment 3:
By the silicon-dioxide (SiO of particle diameter 1-2 μm
2) to add concentration to be, in the Resorcinol of 0.1mol/L and the ethanolic soln of hexanediamine, under magnetic stirrer, react 36h to microballoon, then centrifugal; By obtained PCA@SiO
2particulate utilizes ultrasonic dispersion to be dispersed in the perfluor octylame ethanolic soln of 0.01mol/L 0.5 hour, then vacuum-drying at 40 DEG C, i.e. the obtained poly-phenol amine particulate with ultra-hydrophobicity.
Embodiment 4:
The multi-walled carbon nano-tubes (CNTs) of length 5-15 μm of diameter 20-40nm is added in the pyrocatechol and hexanediamine solution that concentration is 0.2mol/L, under magnetic stirrer, reacts 48h, centrifugal; Ultrasonic dispersion is utilized by obtained PCA@CNTs particulate to be dispersed in the perfluor octylame ethanolic soln of 0.05mol/L 1 hour, then vacuum-drying at 30 DEG C, i.e. the obtained poly-phenol amine particulate with ultra-hydrophobicity.
Claims (8)
1. a preparation method for the super-hydrophobic particulate of poly-phenol amine, is characterized in that: following steps:
(1) micro Nano material is joined in the solution of polyphenol and polyamines, be separated after reaction certain hour, the micro Nano material that obtained poly-phenol is amine-modified;
(2) step (1) gained is gathered the solution that the amine-modified micro Nano material of phenol is scattered in low-surface energy substance, be separated after reaction certain hour, the particulate with ultra-hydrophobicity can be obtained.
2. the preparation method of the super-hydrophobic particulate of a kind of poly-phenol amine as claimed in claim 1, is characterized in that: described micro Nano material is at least one in silicon-dioxide, titanium dioxide, aluminum oxide, zinc oxide, polymer microballoon, carbon nanotube.
3. the preparation method of the super-hydrophobic particulate of a kind of poly-phenol amine as claimed in claim 1, is characterized in that: described polyphenol is at least one in pyrocatechol, Resorcinol.
4. the preparation method of the super-hydrophobic particulate of a kind of poly-phenol amine as claimed in claim 1, is characterized in that: described polyamines is phenylenediamine or structural formula is NH
2(CH
2)
nnH
2aliphatic amide, n represents the integer of 6 to 30, at least one.
5. the preparation method of the super-hydrophobic particulate of a kind of poly-phenol amine as claimed in claim 1, is characterized in that: the mass ratio of described micro Nano material and polyphenol is 1: 0.02 ~ 1.
6. the preparation method of the super-hydrophobic particulate of a kind of poly-phenol amine as claimed in claim 1, is characterized in that: the molar mass ratio of described polyphenol and diamines is 1: 0.9 ~ 1.1.
7. the preparation method of the super-hydrophobic particulate of a kind of poly-phenol amine as claimed in claim 1, is characterized in that: the mass ratio of the micro Nano material that described poly-phenol is amine-modified and low-surface energy substance is 1: 0.1 ~ 1.1.
8. the preparation method of the super-hydrophobic particulate of a kind of poly-phenol amine as claimed in claim 1, it is characterized in that described low-surface energy substance is at least one in long-chain fat amine, long-chain fat mercaptan, perfluoroalkyl amine, wherein long-chain fat amine structure formula is CH
3(CH
2)
nnH
2, n represents the integer of 9 to 30, and long-chain fat mercaptan structural formula is CH
3(CH
2)
nsH, n represent the integer of 9 to 30, and perfluoroalkyl amine structure formula is CF
3(CF
2)
n(CH
2)
mnH
2, n represents the integer of 5 to 10, and m represents the integer of 1 to 2.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108940231A (en) * | 2018-07-05 | 2018-12-07 | 中科广化（重庆）新材料研究院有限公司 | The melamine sponge water-oil separating material and preparation method of a kind of modification of poly-dopamine and application |
| CN109092274A (en) * | 2018-10-25 | 2018-12-28 | 齐鲁工业大学 | A kind of adsorbed film and preparation method of quick heavy-metal ion removal |
| CN109336120A (en) * | 2018-10-12 | 2019-02-15 | 安庆北化大科技园有限公司 | Nano-meter SiO_2 with surface migration2The preparation method and Nano-meter SiO_2 of microballoon2 |
| CN110862592A (en) * | 2019-11-28 | 2020-03-06 | 北京石油化工学院 | Alumina/carboxylic butyronitrile composite material and preparation method thereof |
| CN111777872A (en) * | 2020-06-16 | 2020-10-16 | 嘉兴市轩禾园艺技术有限公司 | Preparation method of functional film for shielding infrared rays |
| CN111995431A (en) * | 2020-08-21 | 2020-11-27 | 东南大学 | Polyphenol amine concrete protective agent material and preparation method thereof |
| CN113045903A (en) * | 2021-04-27 | 2021-06-29 | 北京石油化工学院 | Self-healing polysiloxane dielectric elastomer composite material and preparation method thereof |
| CN114574001A (en) * | 2020-11-30 | 2022-06-03 | 北京化工大学 | Method for preparing hydrophilic carbon black through biomimetic modification of phenolic amine and hydrophilic carbon black |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108940231A (en) * | 2018-07-05 | 2018-12-07 | 中科广化（重庆）新材料研究院有限公司 | The melamine sponge water-oil separating material and preparation method of a kind of modification of poly-dopamine and application |
| CN109336120A (en) * | 2018-10-12 | 2019-02-15 | 安庆北化大科技园有限公司 | Nano-meter SiO_2 with surface migration2The preparation method and Nano-meter SiO_2 of microballoon2 |
| CN109336120B (en) * | 2018-10-12 | 2022-09-09 | 安庆北化大科技园有限公司 | Nano SiO with surface migration 2 Preparation method of microsphere and nano SiO 2 |
| CN109092274A (en) * | 2018-10-25 | 2018-12-28 | 齐鲁工业大学 | A kind of adsorbed film and preparation method of quick heavy-metal ion removal |
| CN109092274B (en) * | 2018-10-25 | 2021-07-30 | 齐鲁工业大学 | Adsorption film for rapidly removing heavy metal ions and preparation method thereof |
| CN110862592A (en) * | 2019-11-28 | 2020-03-06 | 北京石油化工学院 | Alumina/carboxylic butyronitrile composite material and preparation method thereof |
| CN110862592B (en) * | 2019-11-28 | 2022-05-20 | 北京石油化工学院 | Alumina/carboxylic butyronitrile composite material and preparation method thereof |
| CN111777872A (en) * | 2020-06-16 | 2020-10-16 | 嘉兴市轩禾园艺技术有限公司 | Preparation method of functional film for shielding infrared rays |
| CN111995431A (en) * | 2020-08-21 | 2020-11-27 | 东南大学 | Polyphenol amine concrete protective agent material and preparation method thereof |
| CN114574001A (en) * | 2020-11-30 | 2022-06-03 | 北京化工大学 | Method for preparing hydrophilic carbon black through biomimetic modification of phenolic amine and hydrophilic carbon black |
| CN114574001B (en) * | 2020-11-30 | 2023-04-28 | 北京化工大学 | Method for preparing hydrophilic carbon black through biomimetic modification of phenolic amine and hydrophilic carbon black |
| CN113045903A (en) * | 2021-04-27 | 2021-06-29 | 北京石油化工学院 | Self-healing polysiloxane dielectric elastomer composite material and preparation method thereof |
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