CN112266713A - Lanthanum oxide super-hydrophobic polyurethane coating prepared by adopting spraying method - Google Patents
Lanthanum oxide super-hydrophobic polyurethane coating prepared by adopting spraying method Download PDFInfo
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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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
- B05D5/08—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain an anti-friction or anti-adhesive surface
- B05D5/083—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain an anti-friction or anti-adhesive surface involving the use of fluoropolymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/44—Polycarbonates
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
- C08G18/751—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
- C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
- C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
- C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
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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
- 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
- C09D7/61—Additives non-macromolecular inorganic
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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
- C08K2003/221—Oxides; Hydroxides of metals of rare earth metal
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Abstract
The invention discloses a lanthanum oxide super-hydrophobic polyurethane coating prepared by a spraying method, which relates to the technical field of high polymer materials, and the preparation method comprises the following steps: (1) preparing polyurethane, namely, taking a proper amount of polycarbonate polyol, carrying out vacuum dehydration, dissolving the polycarbonate polyol in acetone, reacting the polycarbonate polyol with a proper amount of isophorone diisocyanate under the catalysis of dibutyltin dilaurate to obtain a polyurethane prepolymer, and adding perfluorooctanol into the polyurethane prepolymer to introduce a fluorine-containing chain segment for reaction; (2) doping lanthanum oxide nano particles, namely doping 10% of lanthanum oxide nano particles into the prepared polyurethane emulsion and performing ultrasonic treatment; (3) and (3) filling the treated polyurethane doped with the lanthanum oxide nanoparticles into a small spray bottle, spraying the polyurethane on a base material, gradually heating in an oven, and standing to obtain a finished product. The super-hydrophobic polyurethane coating is invented through a spraying method, the preparation method and conditions are simple and convenient, the prepared lanthanum oxide super-hydrophobic polyurethane coating is easy to repair, strong in hydrophobicity and not easy to oxidize, and is suitable for large-scale application.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a lanthanum oxide super-hydrophobic polyurethane coating prepared by a spraying method.
Background
Polyurethane (PU) coatings have many excellent properties and are widely used in various fields, and superhydrophobic surfaces have been used in the fields of self-cleaning, snow and ice protection, corrosion protection, microfluidics, chemical shielding, oil-water separation, biomedicine, and the like. More and more superhydrophobic surfaces are being investigated for large scale applications.
The general coating polyurethane is not waterproof, is easy to be oxidized and yellow after being used, is easy to swell after absorbing water, is not acid-base resistant, and has shorter service life.
The polyurethane super-hydrophobic coating has the characteristics of good elasticity, high elongation, high strength, outstanding wear resistance, excellent acid resistance, alkali resistance, low temperature resistance, water resistance, good toughness and the like, and the excellent characteristics enable the polyurethane super-hydrophobic coating to be widely applied. The super-hydrophobic surface mainly comprises low surface energy and a micro-nano structure. The micro-nano structure is easily damaged by external influence. In a plurality of preparation methods, the method for repairing the super-hydrophobic surface inevitably has the problems of complex method, instrument use limitation and the like. The invention aims to prepare the super-hydrophobic coating by using a spraying method, and the spraying method is simple and quick and has wide application range.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides the lanthanum oxide super-hydrophobic polyurethane coating prepared by the spraying method, and the lanthanum oxide super-hydrophobic polyurethane coating is not limited to a small-area substrate and a smooth material surface by the spraying method and is also suitable for coating various substrates. If the coating is damaged, the repairing method is simpler and more convenient compared with other methods, and the damaged coating can be repaired at any time and any place.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a lanthanum oxide super-hydrophobic polyurethane coating prepared by a spraying method comprises the following steps:
I. preparation of Polyurethane (PU):
taking 3-8 g of polycarbonate polyol (PCDL: M ═ 2000), dehydrating in vacuum at 70-80 ℃ for 3-5 h, dissolving in 40g of acetone after dehydration, and reacting with 2-5 g of isophorone diisocyanate (IPDI) under the catalysis of 0.1-0.3 g of dibutyltin Dilaurate (DBTL) to obtain a polyurethane prepolymer; 2.5-3.5 g of perfluorooctanol is added to introduce a fluorine-containing chain segment to react for 2-3 hours. Obtaining polyurethane emulsion for later use;
doping of lanthanum oxide nanoparticles:
taking a certain amount of the polyurethane emulsion, and carrying out ultrasonic treatment on the polyurethane emulsion doped with 10-20% of lanthanum oxide nanoparticles for 30-50 min, controlling the temperature by using ice blocks during ultrasonic treatment to avoid side reactions caused by water temperature rise in the ultrasonic process, and filling the treated polyurethane doped with the lanthanum oxide nanoparticles into a small spray bottle for later use;
preparation of superhydrophobic polyurethane:
and (2) spraying the polyurethane doped with the lanthanum oxide nanoparticles on a base material, putting the base material into an oven after spraying, gradually raising the temperature, starting from 20 ℃, raising the temperature by 10 ℃ every hour until the temperature reaches 50 ℃, and standing the base material in the oven for 5 hours to obtain a finished product.
Further, the base material in step III can be selected from various materials with unlimited smoothness, flatness and area.
Compared with the prior art, the invention has the following advantages and beneficial effects:
the super-hydrophobic polyurethane coating is prepared by adopting a spraying method, has good waterproofness, is not easy to oxidize and yellow, has strong hydrophobicity, is not easy to swell after absorbing water, has strong acid and alkali resistance, and has long service life due to the comprehensive properties. The spraying method is not limited to small-area base materials and smooth material surfaces, and is also suitable for coating various base materials. If the coating is damaged, the repairing method is simpler and more convenient compared with other methods, and the damaged coating can be repaired at any time and any place. The invention is suitable for large-scale application because of excellent product performance, wide application scene, low requirement on preparation environment and easy repair and maintenance.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is an electron microscope scan of a paint sample made in accordance with the present invention;
FIG. 2 is an infrared spectrum obtained from a sample tested using an infrared spectrometer;
FIG. 3 is a graph showing the analysis of 2ul water contact angle.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
a lanthanum oxide super-hydrophobic polyurethane coating prepared by a spraying method comprises the following steps:
I. preparation of Polyurethane (PU):
taking 3g of polycarbonate polyol (PCDL: M ═ 2000), dehydrating for 3h under vacuum at 70 ℃, dissolving in 40g of acetone after dehydration, and reacting with 2g of isophorone diisocyanate (IPDI) under the catalysis of 0.1g of dibutyltin Dilaurate (DBTL) to obtain a polyurethane prepolymer; 2.5g of perfluorooctanol is added to introduce a fluorine-containing chain segment for reaction for 2 hours. Obtaining polyurethane emulsion for later use;
doping of lanthanum oxide nanoparticles:
taking a certain amount of the polyurethane emulsion, and carrying out ultrasonic treatment on the polyurethane emulsion doped with 10% of lanthanum oxide nanoparticles for 30min, controlling the temperature by using ice blocks during ultrasonic treatment to avoid side reaction caused by water temperature rise in the ultrasonic process, and filling the treated polyurethane doped with the lanthanum oxide nanoparticles into a small spray bottle for later use;
preparation of superhydrophobic polyurethane:
spraying the polyurethane doped with the lanthanum oxide nanoparticles on a glass plate substrate, putting the glass plate substrate into an oven after spraying, gradually increasing the temperature, starting from 20 ℃, increasing the temperature by 10 ℃ every hour until the temperature reaches 50 ℃, and then standing the glass plate substrate in the oven for 5 hours to obtain a finished product.
Example 2:
a lanthanum oxide super-hydrophobic polyurethane coating prepared by a spraying method comprises the following steps:
I. preparation of Polyurethane (PU):
5g of polycarbonate polyol (PCDL: M ═ 2000) is dehydrated for 4h in vacuum at 75 ℃, and then dissolved in 40g of acetone after dehydration, and reacts with 3g of isophorone diisocyanate (IPDI) under the catalysis of 0.2g of dibutyltin Dilaurate (DBTL) to obtain a polyurethane prepolymer; 3g of perfluorooctanol is added to introduce a fluorine-containing chain segment for reaction for 3 hours. Obtaining polyurethane emulsion for later use;
doping of lanthanum oxide nanoparticles:
taking a certain amount of the polyurethane emulsion, carrying out ultrasonic treatment on 13% doped lanthanum oxide nanoparticles for 40min, controlling the temperature by using ice blocks during ultrasonic treatment to avoid side reaction caused by water temperature rise in the ultrasonic process, and filling the treated polyurethane doped with the lanthanum oxide nanoparticles into a small spray bottle for later use;
preparation of superhydrophobic polyurethane:
spraying the polyurethane doped with the lanthanum oxide nanoparticles on a glass plate substrate, putting the glass plate substrate into an oven after spraying, gradually increasing the temperature, starting from 20 ℃, increasing the temperature by 10 ℃ every hour until the temperature reaches 50 ℃, and then standing the glass plate substrate in the oven for 5 hours to obtain a finished product.
Example 3:
a lanthanum oxide super-hydrophobic polyurethane coating prepared by a spraying method comprises the following steps:
I. preparation of Polyurethane (PU):
taking 8g of polycarbonate polyol (PCDL: M ═ 2000), dehydrating in vacuum at 80 ℃ for 5h, dissolving in 40g of acetone after dehydration, and reacting with 5g of isophorone diisocyanate (IPDI) under the catalysis of 0.3g of dibutyltin Dilaurate (DBTL) to obtain a polyurethane prepolymer; 3.5g of perfluorooctanol is added to introduce a fluorine-containing chain segment for reaction for 3 hours. Obtaining polyurethane emulsion for later use;
doping of lanthanum oxide nanoparticles:
taking a certain amount of the polyurethane emulsion, and carrying out ultrasonic treatment for 50min by doping 20% of lanthanum oxide nanoparticles, controlling the temperature by using ice blocks during ultrasonic treatment to avoid side reaction caused by water temperature rise in the ultrasonic process, and filling the treated polyurethane doped with the lanthanum oxide nanoparticles into a small spray bottle for later use;
preparation of superhydrophobic polyurethane:
and (2) spraying the polyurethane doped with the lanthanum oxide nanoparticles on a glass plate, putting the glass plate into an oven after spraying, gradually raising the temperature, starting from 20 ℃, raising the temperature by 10 ℃ every other hour until the temperature reaches 50 ℃, and standing the glass plate in the oven for 5 hours to obtain a finished product.
Example 4:
a lanthanum oxide super-hydrophobic polyurethane coating prepared by a spraying method comprises the following steps:
I. preparation of Polyurethane (PU):
5g of polycarbonate polyol (PCDL: M ═ 2000) is dehydrated in vacuum at 75 ℃ for 3h, the dehydrated polycarbonate polyol is dissolved in 40g of acetone, and the dehydrated polycarbonate polyol and 3g of isophorone diisocyanate (IPDI) react under the catalysis of 0.2g of dibutyltin Dilaurate (DBTL) to obtain a polyurethane prepolymer; 3g of perfluorooctanol is added to introduce a fluorine-containing chain segment for reaction for 3 hours. Obtaining polyurethane emulsion for later use;
doping of lanthanum oxide nanoparticles:
taking a certain amount of the polyurethane emulsion, carrying out ultrasonic treatment on the polyurethane emulsion doped with 15% of lanthanum oxide nanoparticles for 40min, controlling the temperature by using ice blocks during ultrasonic treatment to avoid side reaction caused by water temperature rise in the ultrasonic process, and filling the treated polyurethane doped with the lanthanum oxide nanoparticles into a small spray bottle for later use;
preparation of superhydrophobic polyurethane:
spraying the polyurethane doped with the lanthanum oxide nanoparticles on a glass plate substrate, putting the glass plate substrate into an oven after spraying, gradually increasing the temperature, starting from 20 ℃, increasing the temperature by 10 ℃ every hour until the temperature reaches 50 ℃, and then standing the glass plate substrate in the oven for 5 hours to obtain a finished product.
Example 5:
and observing the prepared lanthanum oxide super-hydrophobic polyurethane coating under an electron microscope. The construction of superhydrophobic surfaces requires two conditions, low surface energy and micro-nano-scale roughness. The roughness affects the magnitude of the contact angle. As can be seen by an electron microscope (figure 1), the surface of the synapse is provided with micron-sized synapses, the surface of the synapse is not smooth and has a certain rough structure, and the construction of a super-hydrophobic condition is facilitated.
Example 6:
the samples were tested using an infrared spectrometer model Nicolet IS50 thermodissher USA, part number of the molecular spectroscopy section of the american thermal electric group, and the composition of the samples was quantified qualitatively. After grinding and tabletting KBr powder, the sample was directly measured by dropping on the top. On the infrared spectrogram (FIG. 2), the transmission rate (unit%) is shown on the y-axis, and the wave number (unit cm) is shown on the x-axis-1) In the figure, 1240 and 1030 represent C — F stretch, 1740 represents C ═ O stretch (F-PU synthesis) of saturated fatty acids, 640 represents a characteristic La — O peak, and 3370 represents NH stretch (IPDI reaction completed), and La (oh)3 was produced (successful synthesis of fluorine-containing hyperbranched polyurethane). The successful doping of the lanthanum oxide nanoparticles is demonstrated.
Example 7:
the contact angle of the prepared sample was 157 ° using the goniometry (fig. 3), and it is known that the hydrophobicity of the general coating is mainly judged by the size of the contact angle, and in general, we refer to the contact angle less than 60 degrees as the hydrophilic contact angle, and the contact angle more than 60 degrees as the hydrophobic contact angle. The larger the contact angle, the better the hydrophobicity is indicated, so the hydrophobicity of the sample can be proved to be good accordingly.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (2)
1. The lanthanum oxide super-hydrophobic polyurethane coating prepared by a spraying method is characterized by comprising the following steps:
I. preparation of Polyurethane (PU):
taking 3-8 g of polycarbonate polyol (PCDL: M ═ 2000), dehydrating in vacuum at 70-80 ℃ for 3-5 h, dissolving in 40g of acetone after dehydration, and reacting with 2-5 g of isophorone diisocyanate (IPDI) under the catalysis of 0.1-0.3 g of dibutyltin Dilaurate (DBTL) to obtain a polyurethane prepolymer; 2.5-3.5 g of perfluorooctanol is added to introduce a fluorine-containing chain segment to react for 2-3 hours. Obtaining polyurethane emulsion for later use;
doping of lanthanum oxide nanoparticles:
taking a certain amount of the polyurethane emulsion, and carrying out ultrasonic treatment on the polyurethane emulsion doped with 10-20% of lanthanum oxide nanoparticles for 30-50 min, controlling the temperature by using ice blocks during ultrasonic treatment to avoid side reactions caused by water temperature rise in the ultrasonic process, and filling the treated polyurethane doped with the lanthanum oxide nanoparticles into a small spray bottle for later use;
preparation of superhydrophobic polyurethane:
and (2) spraying the polyurethane doped with the lanthanum oxide nanoparticles on a base material, putting the base material into an oven after spraying, gradually raising the temperature, starting from 20 ℃, raising the temperature by 10 ℃ every hour until the temperature reaches 50 ℃, and standing the base material in the oven for 5 hours to obtain a finished product.
2. The lanthanum oxide super-hydrophobic polyurethane coating prepared by the spraying method as claimed in claim 1, wherein the substrate in step III can be selected from various materials with unlimited smoothness, flatness and area.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011085156.6A CN112266713A (en) | 2020-10-12 | 2020-10-12 | Lanthanum oxide super-hydrophobic polyurethane coating prepared by adopting spraying method |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103555184A (en) * | 2013-10-23 | 2014-02-05 | 三棵树涂料股份有限公司 | Super-amphiphobic nano composite finish varnish, and preparation method thereof |
| CN110845952A (en) * | 2019-12-02 | 2020-02-28 | 西北工业大学 | Fluorinated polyurethane coating and preparation method of super-hydrophobic coating |
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2020
- 2020-10-12 CN CN202011085156.6A patent/CN112266713A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103555184A (en) * | 2013-10-23 | 2014-02-05 | 三棵树涂料股份有限公司 | Super-amphiphobic nano composite finish varnish, and preparation method thereof |
| CN110845952A (en) * | 2019-12-02 | 2020-02-28 | 西北工业大学 | Fluorinated polyurethane coating and preparation method of super-hydrophobic coating |
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Application publication date: 20210126 |
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| RJ01 | Rejection of invention patent application after publication |