CN107325718B - Containing nano modified material - Google Patents
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- CN107325718B CN107325718B CN201610586112.9A CN201610586112A CN107325718B CN 107325718 B CN107325718 B CN 107325718B CN 201610586112 A CN201610586112 A CN 201610586112A CN 107325718 B CN107325718 B CN 107325718B
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- 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
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/36—After-treatment
- C08J9/40—Impregnation
- C08J9/405—Impregnation with polymerisable compounds
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
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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
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/085—Copper
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2248—Oxides; Hydroxides of metals of copper
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention discloses a nano-containing modified material, which mainly solves the problems of poor hydrophobic property and poor stability of the modified material in the prior art. The invention solves the problems by adopting the technical scheme that the nano-modified material is dissolved in the hydrophobic organic silicon compound preparation agent and is stirred to be completely dissolved to obtain the nano-modified material, and the nano-modified material can be used for modifying the nano-material.
Description
Technical Field
The invention relates to a material containing nano-modification.
Background
The wettability of a solid surface is generally determined by the chemical composition and the micro-geometry of the surface. In recent years, due to its wide application prospect in industrial and agricultural production and daily life of man and woollen cloth, the super-hydrophobic surface has the following characteristics: the coating has attracted general attention of people gradually, such as oil-water separation, corrosion resistance, self-cleaning, water resistance, antifouling, drag reduction coating and the like. The super-hydrophobic surface generally refers to a surface with a contact angle with water of more than 150 degrees, and in general, the super-hydrophobic surface can be realized by constructing a rough structure on the surface of a hydrophobic material or modifying a low-surface-energy substance on the surface of a solid.
Although many compositions and preparation means and methods of the superhydrophobic modifier have been reported at present, practical application thereof to the formation of the superhydrophobic surface has not been popularized yet, and particularly, a simple, economical, and environmentally-friendly preparation method has yet to be developed. Most of the prior reports on the preparation process of the superhydrophobic surface modifier relate to the reduction of the surface energy of the surface by using expensive low-surface-energy substances, such as compounds containing epoxy resin, dopamine, organic fluorine or organosilicon materials, and the materials also have the defects of poor temperature change adaptability and the like. Moreover, many methods of constructing rough hydrophobic surfaces, such as electrochemical deposition, sol-gel processes, photolithography, layer-by-layer self-assembly, etc., involve specific equipment, harsh conditions and long periods, which are difficult to use for the preparation of low-cost large-scale superhydrophobic materials (CN 104449357 a,2015.03.25, full text; CN 103623709 b,2015.07.01, full text; CN 103305122 b,2015.10.21, full text; CN 102766269 a,2012.11.07, full text; CN 103951843 a,2014.07.30, full text; CN 102619093 b,2014.05.21, full text). In contrast, fluorosilicone polymers, siloxane polymers and the like have low surface energy, have environmental-friendly, temperature change resistance, radiation resistance and excellent recycling stability, can be grafted and polymerized under mild preparation conditions, are firmly loaded on the surface of a modified solid material, are low in price and are suitable for large-area coating. By combining the inherent high specific surface characteristics of the nano particle assistant and the like, coarse structures such as micro-nano protrusions and grooves can be formed on the surface of the solid material, so that the original solid-liquid contact phase is partially replaced by the intercepted air to form a solid-liquid-gas three-phase contact surface, the solid-liquid contact surface is reduced, liquid drops roll off more easily, and finally a super-hydrophobic surface is formed.
Disclosure of Invention
The invention aims to solve the technical problems of poor hydrophobic property and poor stability of a modified material in the prior art, and provides a novel nano-containing modified material. The method has the advantages of high stability and high hydrophobicity.
The technical scheme adopted by the invention is as follows: dissolving a nano material in a hydrophobic organic silicon compound preparation agent, and stirring until the nano material is completely dissolved to obtain the nano modified material; wherein the nano material is selected from carbon-based, copper group metal oxide or nano particles, nano wires or nano belts of silicon dioxide; the hydrophobic organosilicon compound preparation is a toluene cyclohexanone solution of dimethyl siloxane mixed ring DMC or an ethanol solution containing vinyl chlorosilane.
In the above technical solution, preferably, the carbon-based nanoparticles are carbon nanotubes.
In the above technical solution, preferably, the copper group metal-based nanoparticles are ultra-long copper nanowires.
In the above technical solution, preferably, the copper group metal oxide nanoparticles are hyperbranched copper oxide nanorods.
In the above technical solution, preferably, the mass ratio of the nanomaterial to the hydrophobic organosilicon compound formulation is 0.05 to 0.2.
In the above technical scheme, preferably, the compounding ratio of the dimethyl siloxane mixed ring DMC and the nano material is 1-6.
In the above technical scheme, preferably, the mass ratio of the vinyl chlorosilane to the nano material is 0.25-1; the concentration of the vinyl chlorosilane ethanol solution is 3 mg/mL-8 mg/mL.
In the above technical solution, preferably, the mechanical stirring time is more than 4 hours.
The nano modifier stock solution has high adhesive force, and the rough secondary structures constructed on the surface of the solid material are arranged randomly, so that the nano modifier stock solution can bear certain damage and keep good super-hydrophobic performance, and meanwhile, the stock solution has low manufacturing cost, is non-toxic and environment-friendly and is easy to expand the application scale.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) characterization result of the surface of a nano modifier stock solution modified product obtained in example 1;
FIG. 2 is a photograph of the sponge product after modification in example 1 in contact with water droplets;
FIG. 3 shows the results of testing the stability of the modified sponge material obtained in example 1 after 30 times of oil-water separation and recycling;
FIG. 4 shows TEM representation of the nano-modifier dope obtained in example 7;
FIG. 5 is a photograph of the angle of wetting with water of the modified sponge material of example 7;
FIG. 6 is an SEM photograph of the surface of a modified sponge base obtained in example 8;
FIG. 7 shows TEM characterization of the nano-modifier dope obtained in example 9;
FIG. 8 is an SEM photograph of the surface microstructure of the modified sponge base material obtained in example 10;
the present invention will be further illustrated by the following examples, but is not limited to these examples.
Detailed Description
[ example 1 ]
(1) Weighing 2 g of hydrophobic fumed silica nanoparticles and 8.2 g of dimethyl siloxane mixed ring DMC, dissolving in 200 ml of toluene cyclohexanone, placing in a single-neck flask, and mechanically stirring by using a stirring rod for 6 hours until the hydrophobic fumed silica nanoparticles and the dimethyl siloxane mixed ring DMC are dissolved to obtain a modifier stock solution.
(2) And (3) soaking the polyurethane sponge base material in the modifier stock solution for 12 hours, removing and drying, and then putting the polyurethane sponge base material in a 120 ℃ oven to harden for 6 hours to obtain the super-hydrophobic modified sponge material.
Fig. 1 is a scanning electron microscope representation of the sponge material obtained in example 1 before and after surface modification, and observation shows that a large number of nanoparticles are coated on the surface of the modified sample, and the nanoparticle clusters accumulated together form a micro-nano structure and uneven folds, thereby greatly improving the surface roughness of the substrate material; FIG. 2 is a photograph of the sponge product after modification in example 1, in contact with water droplets, showing that the surface has a wetting angle with water of >150 ° and excellent superhydrophobic property; FIG. 3 is a result of 30 oil-water separation cycle tests on the product obtained in example 1, which proves that the stock solution modified base material has excellent stability.
[ example 2 ]
(1) Weighing 1 g of hydrophobic fumed silica nanoparticles and 11.2 g of dimethyl siloxane mixed ring DMC, dissolving in 500 ml of toluene cyclohexanone, placing in a single-neck flask, and mechanically stirring for 4 hours by using a stirring rod until the materials are dissolved to obtain the material containing the nano modified material.
(2) And (3) soaking the polyurethane sponge base material in the modifier stock solution for 12 hours, removing and drying, and then putting the polyurethane sponge base material in a 120 ℃ oven to harden for 6 hours to obtain the super-hydrophobic modified sponge material.
The appearance, hydrophobic properties and stability in use of the product were similar to those of the product obtained in example 1.
[ example 3 ]
(1) 20 g of hydrophobic fumed silica nanoparticles and 240 g of dimethyl siloxane mixed ring DMC were weighed and dissolved in 6L of toluene cyclohexanone, placed in a single-neck flask and mechanically stirred with a stirring rod for 5 hours until dissolved, to obtain the material containing nano-modifications.
(2) And (3) soaking the polyurethane sponge base material in the modifier stock solution for 12 hours, removing and drying, and then putting the polyurethane sponge base material in a 120 ℃ drying oven to harden for 6 hours to obtain the super-hydrophobic modified sponge material.
The appearance, hydrophobic property and cycling stability of the obtained product are similar to those of the product obtained in example 1, which shows that the stock solution can still keep good modification capability after being amplified and produced.
[ example 4 ]
(1) Weighing 2 g of super-hydrophobic silica nanoparticles and 0.6 g of vinyl chlorosilane, dissolving the nano-hydrophobic silica nanoparticles and the vinyl chlorosilane in 200 ml of ethanol, and stirring the mixture for 4 hours to obtain a modifier stock solution.
(2) And (3) soaking the sponge substrate material in the modified solution for 12 hours, taking out, and drying at room temperature for 3 hours to obtain the super-hydrophobic sponge sample.
The appearance, hydrophobic properties and stability in use of the product were similar to those of the product obtained in example 1.
[ example 5 ] A method for producing a polycarbonate
(1) 0.6 g of super-hydrophobic silica nano-particles and 0.6 g of vinyl chlorosilane are weighed and dissolved in 100 ml of ethanol, and magnetons are stirred for 4 hours to obtain a modifier stock solution.
(2) And (3) soaking the sponge substrate material in the modified solution for 12 hours, taking out, and drying at room temperature for 3 hours to obtain the super-hydrophobic sponge sample.
The appearance, hydrophobic properties and stability in use of the product were similar to those of the product obtained in example 1.
[ example 6 ] A method for producing a polycarbonate
(1) Weighing 12 g of super-hydrophobic silica nanoparticles and 6 g of vinyl chlorosilane, dissolving the nano-hydrophobic silica nanoparticles and the vinyl chlorosilane in 800 ml of ethanol, and stirring magnetons for 4 hours to obtain a modifier stock solution.
(2) And (3) soaking the sponge substrate material in the modified solution for 12 hours, taking out, and drying at room temperature for 3 hours to obtain the super-hydrophobic sponge sample.
The appearance, hydrophobic properties and stability in use of the product were similar to those of the product obtained in example 1.
[ example 7 ] A method for producing a polycarbonate
(1) Weighing 2 g of carbon nano tube and 0.6 g of vinyl chlorosilane, dissolving the carbon nano tube and the vinyl chlorosilane in 100 ml of ethanol, stirring magnetons for 4 hours and carrying out ultrasonic treatment to obtain the material containing the nano modification.
(2) And (3) soaking the sponge substrate material in the modified solution for 12 hours, taking out, and drying at room temperature for 3 hours to obtain the super-hydrophobic sponge sample.
FIG. 4 is a Transmission Electron Microscope (TEM) photograph of the nano modifier stock solution obtained in example 7, showing that it has good dispersibility in a fluorosilane ethanol solution;
FIG. 5 is a photograph of the product's static wetting angle with water showing the resulting product wetting angle >150 and, in addition, a charcoal black appearance which is different from the products of examples 1-6, but which has hydrophobic properties and stability in use similar to the products of examples 1-6.
[ example 8 ]
(1) Weighing 2 g of ultra-long copper nanowire powder, dissolving 0.6 g of vinyl chlorosilane in 100 ml of ethanol, stirring the mixture for 4 hours by magnetons, and carrying out ultrasonic treatment to obtain the modified material containing the nano particles.
(2) And (3) soaking the sponge substrate material in the modified solution for 12 hours, taking out, and drying at room temperature for 3 hours to obtain the super-hydrophobic sponge sample.
Fig. 6 is an SEM photograph of the surface of the modified sponge base material obtained in example 8, which shows that the copper nanowires are overlapped on the surface thereof to form an uneven nano-mesh structure and nano-groove morphology.
The hydrophobicity and the stability in use of the product of this example are similar to those of example 1.
[ example 9 ]
(1) Weighing 2 g of hyperbranched copper oxide nanorod and 0.6 g of vinyl chlorosilane, dissolving the hyperbranched copper oxide nanorod and the vinyl chlorosilane in 100 ml of ethanol, stirring the mixture for 4 hours by using a magneton, and carrying out ultrasonic treatment to obtain the material containing the nano modified material.
(2) And (3) soaking the sponge substrate material in the modified solution for 12 hours, taking out, and drying at room temperature for 3 hours to obtain the super-hydrophobic sponge sample.
FIG. 7 is a TEM photograph of the nano modifier dope obtained in example 9, showing that it has good dispersibility in a fluorosilane ethanol solution; the hydrophobicity and the stability in use of the product of this example are similar to those of example 1.
[ example 10 ]
(1) Weighing 2 g of silicon dioxide nanobelt and 0.6 g of vinyl chlorosilane, dissolving the mixture in 100 ml of ethanol, stirring the mixture for 4 hours by magnetons, and carrying out ultrasonic treatment to obtain the material containing the nano modified material.
(2) And (3) soaking the sponge substrate material in the modified solution for 12 hours, taking out, and drying at room temperature for 3 hours to obtain the super-hydrophobic sponge sample.
FIG. 8 is an SEM photograph of the surface micro-morphology of the modified sponge base material obtained in example 10, which shows that the silica nanobelt can also form a coarse micro-nano structure on the surface of the base material; the hydrophobicity and the stability in use of the product obtained in this example are similar to those of example 1.
[ example 11 ]
Under the best test condition, the modified sponge materials prepared in examples 1-10 are subjected to a water contact angle test to determine the super-hydrophobic property, and as shown in table 1, the materials obtained by the design and preparation method of the invention all have super-hydrophobic characteristics:
TABLE 1
Claims (1)
1. A preparation method of a super-hydrophobic modified sponge material is characterized by comprising the following steps:
(1) Weighing 2 g of hydrophobic fumed silica nanoparticles and 8.2 g of dimethyl siloxane mixed ring DMC, dissolving in 200 ml of toluene cyclohexanone, placing in a single-neck flask, and mechanically stirring for 6 hours by using a stirring rod until the hydrophobic fumed silica nanoparticles and the dimethyl siloxane mixed ring DMC are dissolved to obtain a modifier stock solution;
(2) And (3) soaking the polyurethane sponge base material in the modifier stock solution for 12 hours, removing and drying, and then putting the polyurethane sponge base material in a 120 ℃ oven to harden for 6 hours to obtain the super-hydrophobic modified sponge material.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20110085591A (en) * | 2010-01-21 | 2011-07-27 | 포항공과대학교 산학협력단 | Method of preparing superhydrophobic surface capable of reversible switching |
| CN104231916A (en) * | 2014-09-30 | 2014-12-24 | 东南大学 | Transparent super-hydrophobic nano-coating and spraying and preparation method thereof |
| CN105176150A (en) * | 2015-10-27 | 2015-12-23 | 华北电力大学（保定） | Preparing method for transparent super-hydrophobic coating resistant to cutting and acid and alkaline corrosion |
| CN105413488A (en) * | 2015-12-11 | 2016-03-23 | 上海交通大学 | Preparation method and application of super-hydrophobic membrane |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| TW201311550A (en) * | 2011-09-14 | 2013-03-16 | Univ Nat Taiwan | Carbon nanotube suspension and superhydrophobic film prepared therefrom |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20110085591A (en) * | 2010-01-21 | 2011-07-27 | 포항공과대학교 산학협력단 | Method of preparing superhydrophobic surface capable of reversible switching |
| CN104231916A (en) * | 2014-09-30 | 2014-12-24 | 东南大学 | Transparent super-hydrophobic nano-coating and spraying and preparation method thereof |
| CN105176150A (en) * | 2015-10-27 | 2015-12-23 | 华北电力大学（保定） | Preparing method for transparent super-hydrophobic coating resistant to cutting and acid and alkaline corrosion |
| CN105413488A (en) * | 2015-12-11 | 2016-03-23 | 上海交通大学 | Preparation method and application of super-hydrophobic membrane |
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| Title |
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| Fabrication of hierarchically structured superhydrophobic PDMS surfaces by Cu and CuO casting;Christopher P et al;《Applied Surface Science》;20150624;第353卷;第269-274页 * |
| 超疏水材料的制备及性能研究;田庆文;《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》;20130315(第3期);第B020-198页 * |
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Effective date of registration: 20221018 Address after: Yanan City, Shandong province Qingdao City three road 266071 No. 218 Applicant after: CHINA PETROLEUM & CHEMICAL Corp. Applicant after: Sinopec Safety Engineering Research Institute Co.,Ltd. Address before: Yanan City, Shandong province Qingdao City three road 266071 No. 218 Applicant before: CHINA PETROLEUM & CHEMICAL Corp. Applicant before: SINOPEC Research Institute OF SAFETY ENGINEERING |
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