CN102604534A - Preparation method of benzoxazine super-hydrophobic conductive coating - Google Patents
Preparation method of benzoxazine super-hydrophobic conductive coating Download PDFInfo
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- CN102604534A CN102604534A CN201210067899XA CN201210067899A CN102604534A CN 102604534 A CN102604534 A CN 102604534A CN 201210067899X A CN201210067899X A CN 201210067899XA CN 201210067899 A CN201210067899 A CN 201210067899A CN 102604534 A CN102604534 A CN 102604534A
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Abstract
The invention relates to a preparation method of benzoxazine super-hydrophobic conductive coating, which includes the following steps of dissolving benzoxazine into solvent, adding ketjen black into solution, sufficiently stirring and uniformly dispersing to obtain dispersing solution. By coating rotationally, spraying and casting solution, the dispersing solution is uniformly applied on the surface of a substrate, heated to be cured in a cross linking manner and cooled to obtain the benzoxazine super-hydrophobic conductive coating. The preparation method is convenient, fine in controllability, low in cost and free of complicated chemical treatment, and the coating is fine in hydrophobicity, static contact angle between the coating and the water is larger than 150 degrees, rolling angle between the same is smaller than 5 degrees, and volume resistivity of the coating is smaller than 102 omega cm. Meanwhile, the coating is fine in alkali and acid resistance and solvent resistance and has wide application prospect.
Description
Technical field
The present invention relates to a kind of preparation method of benzoxazine ultra-hydrophobic conductive coating.
Background technology
It is super-hydrophobic that (the water static contact angle is greater than 150 °; Roll angle is less than 5 °) surface has anti-adhesive, anti-pollution, self-cleaning performance, therefore reduces friction at hull surface, antibiont adheres to aspects such as coating, outdoor antenna, automatically cleaning stop-light, antifouling fabric, oily water separation and has important application prospects.
Continuous progress along with the super hydrophobic surface research work; Various multi-functional super hydrophobic surfaces are continually developed out; Wherein have the super hydrophobic surface of conductivity because its surface has the electric heating effect, and can the static charge that be accumulated in the surface be removed, therefore in the deicing of anti-ice; Waterproofed electronics has the potential using value on the antistatic hydrophobic material.
[Das A, Hayvaci HT, Tiwari MK such as Das; Et al.; Superhydrophobic and conductive carbon nanofiber/PTFE composite coatings for EMI shielding. J. Coll. Interf. Sci. 2011,353 (1), 311-315] to utilize carbon nano-tube fibre and TPFE to prepare contact angle be 158 °; Roll angle is 10 °; The conduction super-hydrophobic coat of specific conductivity 309 S/m, coating has self-cleaning performance, and can be used as electromagnetic shielding material.[Zou JH, Cher H, Chunder H such as Zou; Et al.; Preparation of a superhydrophobic and conductive nanocomposite coating from a carbon-nanotube-conjugated block copolymer dispersion. Adv. Mater. 2008,20 (17), 3337-3341] method through solution-cast prepared the conduction super hydrophobic film; Water contact angle is 154 ~ 160 °, and roll angle is less than 5 ° super hydrophobic surface.Specific conductivity that simultaneously should the surface is in 30 ~ 100S/cm scope.Can be used for detection,, have higher sensitivity so receive influence of moisture littler than general test material owing to have superhydrophobic property to organic gas.[Peng M such as Peng; Liao ZJ; Qi J; Zhou Z. Nonaligned Carbon Nanotubes Partially Embedded in Polymer Matrixes:A Novel Route to Superhydrophobic Conductive Surfaces. Langmuir. 2010,26 (16), 13572-13578] introduced pressure sintering has super-hydrophobicity and high conductivity in the multiple polymers surface preparation compound coating.The water contact angle of compound coating is about 160 °, and in 2.0 ~ 4.5 ° of scopes, the surface has very high electroconductibility for different matrix roll angles, and square resistance is lower than 10
3Ω/sq.Through fluoroalkyl silanes multi-walled carbon nano-tubes (MWNTs) is carried out surface-treated and can improve super-hydrophobic stability.
Use expensive low surface energy material but all relate in the preparation process of most of super hydrophobic surfaces of existing report, reduce the surface energy on surface like the compound of fluorine-containing or silane, and much harmful to human body and environment.Therefore invent a kind of simply, use cheap not fluorine-containing material to prepare the ultra-hydrophobic conductive coating and be necessary.[Wang CF such as Wang; Su YC, Kuo SW, et al.; Low-surface-free-energy materials based on polybenzoxazines. Angew Chem Int Edit. 2006; 45 (14), 2248-51] discover that Polybenzoxazine has lower surface energy (16.4 mJ/m
2), even be lower than tetrafluoroethylene (21 mJ/m
2), and Polybenzoxazine has the preparation advantage cheap and easy to process that tetrafluoroethylene does not possess simultaneously.Have better chemical stability simultaneously, low water absorbable is a kind of ideal low surface energy material.
Summary of the invention
The objective of the invention is that ultra-hydrophobic conductive coating prepn material is more expensive in order to overcome, complicated process of preparation, ultra-hydrophobic conductive property are relatively poor, the defective of resistance to acids and bases and poor solvent resistance, and the preparation method of the benzoxazine ultra-hydrophobic conductive coating that a kind of technology is simple and cost is low, performance is good is provided.
The preparation method of benzoxazine ultra-hydrophobic conductive coating of the present invention may further comprise the steps:
(1) the 0.01-10g benzoxazine is dissolved in the 1-100ml solvent, in benzoxazine solution, adds the 0.01-1g Ketjen black then, fully stir, be uniformly dispersed, obtain dispersion liquid;
(2) adopt the method for spin coating, spraying or solution-cast, the dispersion liquid of step (1) is applied to matrix surface, after 170-250 ℃ of following crosslinking curing 1-6 hour, cooling obtains benzoxazine ultra-hydrophobic conductive coating.
Among the present invention, said benzoxazine is 2, two (the 3-phenyl-3 of 2-; 4-dihydro-2H-1, the 3-benzoxazine) propane, 2, two (the 3-methyl-3 of 2-; 4-dihydro-2H-1, the 3-benzoxazine) propane and 2, two (the 3-allyl groups-3 of 2-; 4-dihydro-2H-1,3-benzoxazine) mixture of one or more in the propane.
Among the present invention, said solvent is THF, toluene, YLENE, acetone, N, the mixture of one or more in dinethylformamide, dioxane and the trichloromethane.
Among the present invention, said Ketjen black is one or both the mixture among Ketjen black EC600JD and the EC300J.
Among the present invention, said matrix is glass, wood chip, pottery, burlap, terylene or polyester film.
Compared with prior art, the invention has the advantages that: method is easy, controllability good, cost is low, need not complex chemical treatment, and gained coating hydrophobicity is good, and the coating volume specific resistance is less than 10
2Ω cm, coating resistance to acids and bases and solvent resistance are good simultaneously.
Description of drawings
Fig. 1 is field emission scanning electron microscope (FE-SEM) photo of benzoxazine ultra-hydrophobic conductive coating at glass surface.
Fig. 2 is the static contact angle optical photograph of benzoxazine ultra-hydrophobic conductive coating at glass surface.
Fig. 3 is field emission scanning electron microscope (FE-SEM) photo of benzoxazine ultra-hydrophobic conductive coating on the wood chip surface.
Fig. 4 is the static contact angle optical photograph of benzoxazine ultra-hydrophobic conductive coating on the wood chip surface.
Embodiment
Below in conjunction with embodiment the present invention is described further, but the invention is not restricted to following examples.
Embodiment 1
With 0.20g 2,2-two (3-phenyl-3,4-dihydro-2H-1; The 3-benzoxazine) propane is dissolved in the 10ml THF, in this solution, adds 0.05g Ketjen black EC600JD then, and magnetic agitation was uniformly dispersed it in 4 hours; Dispersion liquid is spin-coated on glass; Spin coating is 60 seconds under the 1500rpm condition, changes coating over to 190 ℃ of baking ovens and makes its crosslinking curing 6 hours, and cooling obtains benzoxazine ultra-hydrophobic conductive coating.The hydrophobicity of testing coating, with the quiet contact angle average of water be 165 °, roll angle is 2.5 °, the coating volume specific resistance is 26.5 Ω cm.Fig. 1 is a benzoxazine ultra-hydrophobic conductive coatingsurface pattern.Fig. 2 is the static contact angle optical photograph of benzoxazine ultra-hydrophobic conductive coatingsurface.
Embodiment 2
With 0.30g 2,2-two (3-methyl-3,4-dihydro-2H-1; The 3-benzoxazine) propane is dissolved in the 20ml THF, in this solution, adds 0.08g Ketjen black EC600JD, magnetic agitation 4 hours then; It is uniformly dispersed; Dispersion liquid is cast on the wood chip, change 190 ℃ of baking ovens over to and make its crosslinking curing 6 hours, cooling obtains benzoxazine ultra-hydrophobic conductive coating.The hydrophobicity of testing coating, with the quiet contact angle average of water be 168 °, roll angle is 3.5 °, the coating volume specific resistance is 87.2 Ω cm.Fig. 3 is a benzoxazine ultra-hydrophobic conductive coatingsurface pattern.Fig. 4 is the static contact angle optical photograph of benzoxazine ultra-hydrophobic conductive coatingsurface.
Embodiment 3
With 0.50g 2,2-two (3-phenyl-3,4-dihydro-2H-1; The 3-benzoxazine) propane is dissolved in and contains 9ml THF and 1ml N, in the dinethylformamide, in this solution, adds 0.08g Ketjen black EC600JD then; Magnetic agitation was uniformly dispersed it in 4 hours, dispersion liquid was spin-coated on glass, and spin coating is 60 seconds under the 1500rpm condition; Change coating over to 200 ℃ of baking ovens and make its crosslinking curing 6 hours, cooling obtains benzoxazine ultra-hydrophobic conductive coating.The hydrophobicity of testing coating, with the quiet contact angle average of water be 162 °, roll angle is 2.5 °, the coating volume specific resistance is 8.0 Ω cm.
Embodiment 4
With 0.10g 2,2-two (3-allyl group-3,4-dihydro-2H-1; The 3-benzoxazine) propane is dissolved in and contains 40ml THF and 10ml N, in the dinethylformamide, in this solution, adds 0.10g Ketjen black EC300J then; Magnetic agitation was uniformly dispersed it in 4 hours; Dispersion liquid is sprayed on the wood chip, changes 180 ℃ of baking ovens over to and make its crosslinking curing 6 hours, cooling obtains benzoxazine ultra-hydrophobic conductive coating.The hydrophobicity of testing coating, with the quiet contact angle average of water be 151 °, roll angle is 4.5 °, the coating volume specific resistance is 92.5 Ω cm.
Embodiment 5
With 1.00g 2,2-two (3-methyl-3,4-dihydro-2H-1; The 3-benzoxazine) propane is dissolved in the 100ml THF; In this solution, add 0.50g Ketjen black EC300J then, magnetic agitation was uniformly dispersed it in 4 hours, dispersion liquid was cast on glass; Change 240 ℃ of baking ovens over to and make its crosslinking curing 2 hours, cooling obtains benzoxazine ultra-hydrophobic conductive coating.The hydrophobicity of testing coating, with the quiet contact angle average of water be 156 °, roll angle is 3.5 °, the coating volume specific resistance is 56.5 Ω cm.
Embodiment 6
With 0.01g 2,2-two (3-phenyl-3,4-dihydro-2H-1; The 3-benzoxazine) propane is dissolved in the 10ml THF; In this solution, add 0.02g Ketjen black EC300J then, magnetic agitation was uniformly dispersed it in 4 hours, and dispersion liquid is cast on the PET film; Change 170 ℃ of baking ovens over to and make its crosslinking curing 4 hours, cooling obtains benzoxazine ultra-hydrophobic conductive coating.The hydrophobicity of testing coating, with the quiet contact angle average of water be 154 °, roll angle is 4.5 °, the coating volume specific resistance is 36.5 Ω cm.
Embodiment 7
With 0.10g 2,2-two (3-allyl group-3,4-dihydro-2H-1; The 3-benzoxazine) propane is dissolved in and contains 18ml THF and 2ml N, in the dinethylformamide, in this solution, adds 0.20g Ketjen black EC600JD then; Magnetic agitation was uniformly dispersed it in 4 hours, dispersion liquid was spin-coated on glass, and spin coating is 60 seconds under the 1500rpm condition; Change coating over to 200 ℃ of baking ovens and make its crosslinking curing 5 hours, cooling obtains benzoxazine ultra-hydrophobic conductive coating.The hydrophobicity of testing coating, with the quiet contact angle average of water be 158 °, roll angle is 3.5 °, the coating volume specific resistance is 44.8 Ω cm.
Embodiment 8
With 0.20g 2,2-two (3-methyl-3,4-dihydro-2H-1; The 3-benzoxazine) propane is dissolved in and contains 9ml acetone and 1ml N, in the dinethylformamide, in this solution, adds 0.08g Ketjen black EC600JD then; Magnetic agitation was uniformly dispersed it in 4 hours, and dispersion liquid is spin-coated on the PET film, and spin coating is 60 seconds under the 1500rpm condition; Change coating over to 190 ℃ of baking ovens and make its crosslinking curing 6 hours, cooling obtains benzoxazine ultra-hydrophobic conductive coating.The hydrophobicity of testing coating, with the quiet contact angle average of water be 163 °, roll angle is 3.5 °, the coating volume specific resistance is 12.4 Ω cm.
Embodiment 9
With 5.00g 2,2-two (3-phenyl-3,4-dihydro-2H-1; The 3-benzoxazine) propane is dissolved in and contains 90ml acetone and 10ml N, in the dinethylformamide, in this solution, adds 0.50g Ketjen black EC600JD then; Magnetic agitation was uniformly dispersed it in 4 hours; Dispersion liquid is cast on the burlap, change 180 ℃ of baking ovens over to and make its crosslinking curing 6 hours, cooling obtains benzoxazine ultra-hydrophobic conductive coating.The hydrophobicity of testing coating, with the quiet contact angle average of water be 152 °, roll angle is 4.5 °, the coating volume specific resistance is 54.5 Ω cm.
Claims (5)
1. the preparation method of a benzoxazine ultra-hydrophobic conductive coating is characterized in that may further comprise the steps:
(1) the 0.01-10g benzoxazine is dissolved in the 1-100ml solvent, in benzoxazine solution, adds the 0.01-1g Ketjen black then, fully stir, be uniformly dispersed, obtain dispersion liquid;
(2) adopt the method for spin coating, spraying or solution-cast, the dispersion liquid of step (1) is applied to matrix surface, at 170-250 ℃ of following crosslinking curing 1-6 hour, cooling obtained benzoxazine ultra-hydrophobic conductive coating.
2. according to the method for the described benzoxazine ultra-hydrophobic conductive of claim 1 coating, it is characterized in that said benzoxazine is 2, two (the 3-phenyl-3 of 2-; 4-dihydro-2H-1, the 3-benzoxazine) propane, 2, two (the 3-methyl-3 of 2-; 4-dihydro-2H-1, the 3-benzoxazine) propane and 2, two (the 3-allyl groups-3 of 2-; 4-dihydro-2H-1,3-benzoxazine) mixture of one or more in the propane.
3. according to the preparation method of the described benzoxazine ultra-hydrophobic conductive of claim 1 coating; It is characterized in that said solvent is THF, toluene, YLENE, acetone, N, the mixture of one or more in dinethylformamide, dioxane and the trichloromethane.
4. according to the preparation method of the described benzoxazine ultra-hydrophobic conductive of claim 1 coating, it is characterized in that said Ketjen black is one or both the mixture among Ketjen black EC600JD and the EC300J.
5. according to the preparation method of the described benzoxazine ultra-hydrophobic conductive of claim 1 coating, it is characterized in that said matrix is glass, wood chip, pottery, burlap, terylene or polyester film.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106178599A (en) * | 2015-05-06 | 2016-12-07 | 华东理工大学 | A kind of automatically cleaning polybenzoxazine super-hydrophobic super-oleophylic fiber web material and preparation thereof and application in oil-water separation |
| CN111100513A (en) * | 2019-12-27 | 2020-05-05 | 杭州吉华高分子材料股份有限公司 | Preparation method of carbon nanotube composite ceramic network modified water-based non-stick coating |
| CN111876059A (en) * | 2020-08-12 | 2020-11-03 | 四川星利石大涂装材料有限公司 | Super-hydrophobic modified polyurea coating and preparation and application thereof |
| CN113235303A (en) * | 2021-06-08 | 2021-08-10 | 青岛大学 | Polybenzoxazine modified polyphenylene sulfide material and preparation method thereof |
| CN114434997A (en) * | 2022-01-26 | 2022-05-06 | 江苏新光镭射包装材料股份有限公司 | Nickel-free wide-width film pressing film and processing technology thereof |
| WO2023285146A1 (en) * | 2021-07-15 | 2023-01-19 | Rise Research Institutes of Sweden AB | Porous material |
Citations (1)
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| CN101792631A (en) * | 2010-04-01 | 2010-08-04 | 国家电网公司 | High hydrophobic static-electricity conducting anti-icing coating and method for producing same |
-
2012
- 2012-03-15 CN CN201210067899XA patent/CN102604534A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101792631A (en) * | 2010-04-01 | 2010-08-04 | 国家电网公司 | High hydrophobic static-electricity conducting anti-icing coating and method for producing same |
Non-Patent Citations (1)
| Title |
|---|
| CHIH FENG WANG ET AL: "Low-surface-Free-Energy materials Based On Polybenzoxazines", 《ANGEWANDTE CHEMIE-INTERNATIONAL EDITION》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106178599A (en) * | 2015-05-06 | 2016-12-07 | 华东理工大学 | A kind of automatically cleaning polybenzoxazine super-hydrophobic super-oleophylic fiber web material and preparation thereof and application in oil-water separation |
| CN111100513A (en) * | 2019-12-27 | 2020-05-05 | 杭州吉华高分子材料股份有限公司 | Preparation method of carbon nanotube composite ceramic network modified water-based non-stick coating |
| CN111100513B (en) * | 2019-12-27 | 2021-08-03 | 杭州吉华高分子材料股份有限公司 | Preparation method of carbon nanotube composite ceramic network modified water-based non-stick coating |
| CN111876059A (en) * | 2020-08-12 | 2020-11-03 | 四川星利石大涂装材料有限公司 | Super-hydrophobic modified polyurea coating and preparation and application thereof |
| CN113235303A (en) * | 2021-06-08 | 2021-08-10 | 青岛大学 | Polybenzoxazine modified polyphenylene sulfide material and preparation method thereof |
| CN113235303B (en) * | 2021-06-08 | 2023-08-18 | 青岛大学 | Polybenzoxazine modified polyphenylene sulfide material and preparation method thereof |
| WO2023285146A1 (en) * | 2021-07-15 | 2023-01-19 | Rise Research Institutes of Sweden AB | Porous material |
| CN114434997A (en) * | 2022-01-26 | 2022-05-06 | 江苏新光镭射包装材料股份有限公司 | Nickel-free wide-width film pressing film and processing technology thereof |
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Application publication date: 20120725 |