CN108912994B - Preparation method of nitrogen-doped titanium dioxide self-cleaning waterborne polyurethane coating - Google Patents
Preparation method of nitrogen-doped titanium dioxide self-cleaning waterborne polyurethane coating Download PDFInfo
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- CN108912994B CN108912994B CN201810772984.3A CN201810772984A CN108912994B CN 108912994 B CN108912994 B CN 108912994B CN 201810772984 A CN201810772984 A CN 201810772984A CN 108912994 B CN108912994 B CN 108912994B
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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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- 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
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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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
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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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
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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Paints Or Removers (AREA)
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- Application Of Or Painting With Fluid Materials (AREA)
Abstract
The invention discloses a preparation method of a nitrogen-doped titanium dioxide self-cleaning waterborne polyurethane coating, belonging to the field of chemical coatings. The coating comprises the following components: water, polyurethane resin, a nitrogen-doped titanium dioxide photocatalytic self-cleaning agent, a dispersing agent, a curing agent, a defoaming agent, a film-forming auxiliary agent and a flatting agent. The doping of nitrogen element can reduce the forbidden bandwidth of titanium dioxide to a certain extent, and reduce the light energy required by photocatalysis, so that the titanium dioxide can be subjected to photocatalysis under the condition of white light, and the application range of the titanium dioxide is greatly enlarged. Because titanium dioxide has a large number of hydroxyl groups, in the preparation process of mixing the waterborne polyurethane, the hydroxyl groups of the titanium dioxide are easy to react with unreacted isocyanic acid radicals and active chain extension groups in the waterborne polyurethane resin to generate stable chemical bonds, so that the dispersibility of the titanium dioxide powder in the polyurethane emulsion is greatly improved, and the stability of the emulsion is correspondingly improved.
Description
Technical Field
The invention belongs to the field of chemical coatings, and particularly relates to a preparation method of a nitrogen-doped titanium dioxide self-cleaning waterborne polyurethane coating.
Background
The development history of the paint is long, and ancient people in China can use natural grease and resin such as tung oil, rosin and the like to manufacture the paint more than 3000 years ago. Since the eighteenth century, the development of modern natural science and the establishment of organic chemistry lay a solid theoretical foundation for the research of coatings, and the coatings formally board the industrial stage. With the establishment and development of polymer chemistry, coatings begin to gradually move to the synthetic resin era, and functional coatings such as epoxy, amino, nitro, polyester, polyurethane, acrylic acid, organosilicon, fluorocarbon and the like are developed in succession. In the twenty-first century, along with the enhancement of environmental protection consciousness of people, energy use is in tension day by day, and environmental protection, energy conservation and high efficiency are the subjects of the times. The coating is developed towards the direction of energy conservation, resource conservation, no pollution and high efficiency. Therefore, the development of high-efficiency water-based paint is very important.
In the twenty-first century, the goal of scientists is to better solve the two problems of energy shortage and environmental pollution caused by economic development. The titanium dioxide photocatalysis technology has important application prospect in the fields of energy and environment. The titanium dioxide photocatalyst absorbs certain lightThe energy then generates photoelectrons and electron holes, making it redox. The oxidative property of the catalyst can effectively catalyze and degrade Volatile Organic Compounds (VOC) in the environment into CO2And H2O, thereby reducing the pollution to the environment. The nitrogen-doped titanium dioxide is added into the coating, so that the coating is endowed with the functions of air purification, sterilization, disinfection and self-cleaning, and meanwhile, TiO2Also a filler or pigment commonly used in coatings, with TiO being added2The polyurethane coating film layer has good light scattering capability, and the yellowing resistance and the toughness of the polyurethane film layer are greatly improved.
Disclosure of Invention
The invention aims to provide a preparation method of a nitrogen-doped titanium dioxide self-cleaning waterborne polyurethane coating, aiming at the problems of uneven dispersion, low catalytic efficiency and small application range caused by overhigh light energy requirement (needing to be carried out under ultraviolet irradiation) and overlarge titanium dioxide particle size of the existing titanium dioxide photocatalytic self-cleaning agent. The coating can generate photocatalysis under white light, and the photocatalysis self-cleaning effect is more obvious, the self-cleaning capability is strong, and the coating is more durable.
In order to achieve the purpose, the invention is realized by the following technical scheme:
nitrogen-doped titanium dioxide (N-TiO)2) The self-cleaning waterborne polyurethane coating comprises, by weight, 25 ~ 35 parts of water, 50 ~ 60 parts of polyurethane resin, 0.3 ~ 1.0.0 part of nitrogen-doped titanium dioxide photocatalytic self-cleaning agent, 1.5 ~ 2.5.5 parts of dispersing agent, 1 ~ 1.5.5 parts of curing agent, 0.8 ~ 1 part of defoaming agent, 0.5 ~ 0.8.8 part of film-forming assistant and 0.5 ~ 0.8.8 part of flatting agent.
The dispersing agent is a carboxylic acid copolymer salt dispersing agent, the curing agent is a polyamide curing agent, the defoaming agent is an organic silicon defoaming agent, the film-forming assistant is an alcohol ether film-forming assistant, and the flatting agent is a polysiloxane flatting agent.
The preparation method of the nitrogen-doped titanium dioxide photocatalytic self-cleaning agent specifically comprises the following steps:
preparing 5.0 mol/L concentrated sulfuric acid, adding 1 g of TiN powder and 60 ~ 70mL of newly prepared concentrated sulfuric acid into a hydrothermal reaction kettle, adding a stirring magneton (the rotating speed of the stirring magneton is 400 ~ 600 rmp) into the hydrothermal reaction kettle, placing the hydrothermal reaction kettle into an oil bath kettle at 140 ℃ for stirring reaction for 10-16h, taking out the hydrothermal reaction kettle after the reaction is finished, cooling the hydrothermal reaction kettle, washing the hydrothermal reaction kettle with deionized water and ethanol until a washing solution is neutral, and drying the hydrothermal reaction kettle to obtain the nitrogen-doped titanium dioxide photocatalytic self-cleaning agent, wherein the particle size of the nitrogen-doped titanium dioxide photocatalytic self-cleaning agent is 400 ~ 600 nm.
The preparation method of the nitrogen-doped titanium dioxide self-cleaning aqueous polyurethane coating comprises the steps of ultrasonically dispersing nitrogen-doped titanium dioxide photocatalytic self-cleaning agent powder in deionized water for 30min, slowly dripping the dispersion into a reaction system before adding deionized water into a polyurethane prepolymer for emulsification in the preparation process of an aqueous polyurethane emulsion, stirring until the mixture is uniformly mixed, emulsifying, distilling under reduced pressure to remove acetone to obtain a compound of polyurethane resin and the nitrogen-doped titanium dioxide photocatalytic self-cleaning agent powder, uniformly mixing a dispersing agent, a curing agent, a defoaming agent, a film forming aid and a leveling agent in proportion, and uniformly mixing by using a mechanical shearing action.
According to the invention, the nitrogen-doped titanium dioxide is prepared by improving the traditional hydrothermal method and stirring in a hydrothermal reaction kettle. The nitrogen-doped titanium dioxide particles obtained by uniform stirring under hydrothermal conditions have small size and high uniformity, so that the dispersion effect of the nitrogen-doped titanium dioxide particles in the coating is greatly improved, the specific surface area of the small-size nitrogen-doped titanium dioxide particles is correspondingly improved, and the photocatalytic self-cleaning capability is multiplied. The doping of nitrogen element to titanium dioxide reduces the forbidden bandwidth of titanium dioxide to a certain extent, reduces the light energy required by photocatalysis, enables the titanium dioxide to be photocatalytic under the condition of white light, and greatly enlarges the application range. The nitrogen-doped titanium dioxide has a large number of hydroxyl groups, and the nitrogen-doped titanium dioxide is added in the preparation process of the aqueous polyurethane resin, is combined with the polyurethane resin in a semi-chemical semi-physical mode, is not purely physically blended, and the hydroxyl groups in the nitrogen-doped titanium dioxide are easy to react with unreacted isocyanic acid radicals and active chain extension groups in the aqueous polyurethane resin to generate stable chemical bonds, so that the dispersibility of the nitrogen-doped titanium dioxide powder in the polyurethane emulsion is greatly improved, and the stability of the emulsion is correspondingly improved.
The invention has the beneficial effects that:
(1) the photocatalytic self-cleaning coating prepared by the invention has excellent photocatalytic self-cleaning effect and lasting self-cleaning time, and the water-based coating does not contain formaldehyde, mercury and other heavy metals, and has the advantages of no toxicity, no pollution, high water resistance, high weather resistance and high wear resistance.
(2) The invention is different from titanium dioxide prepared under the common hydrothermal condition, the particle size of the titanium dioxide particles can be controlled within 1 micron, the uniformity is better, the specific surface of the titanium dioxide can be improved to a great extent, the utilization rate of photocatalysis is higher, and the effect is more obvious.
(3) The detection of the polyurethane coating film on the degradation rate of methylene blue and the test of a contact angle experiment show that the coating film has the self-cleaning capability.
(4) The invention carries out nitrogen doping on the titanium dioxide, thereby reducing the forbidden bandwidth of the titanium dioxide, reducing the energy required by photocatalysis (required light wave red shift), greatly expanding the application field of the self-cleaning coating, namely, the photocatalysis can be carried out only under the condition of white light.
Drawings
FIG. 1: degradation rates of different materials for methylene blue;
FIG. 2: SEM image of nitrogen-doped titanium dioxide;
FIG. 3: XPS plot of nitrogen-doped titanium dioxide;
FIG. 4: and (3) a contact angle analysis chart of the nitrogen-doped titanium dioxide polyurethane coating film.
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited to these examples.
Example 1
The nitrogen-doped titanium dioxide self-cleaning waterborne polyurethane coating comprises the following raw materials in parts by weight: 25 parts of water, 60 parts of polyurethane resin, 0.4 part of nitrogen-doped titanium dioxide photocatalytic self-cleaning agent, 2.5 parts of dispersing agent, 1 part of curing agent, 0.8 part of defoaming agent, 0.8 part of film-forming assistant and 0.8 part of flatting agent.
The dispersing agent is a carboxylic acid copolymer salt dispersing agent, the curing agent is a polyamide curing agent, the defoaming agent is an organic silicon defoaming agent, the film-forming assistant is an alcohol ether film-forming assistant, and the flatting agent is a polysiloxane flatting agent.
The preparation method of the nitrogen-doped titanium dioxide photocatalytic self-cleaning agent specifically comprises the following steps:
preparing the nitrogen-doped titanium dioxide photocatalytic self-cleaning agent by adopting an improved hydrothermal method: preparing 5.0 mol/L concentrated sulfuric acid, and adding 1 g of TiN powder and 70mL of fresh concentrated sulfuric acid into a hydrothermal reaction kettle. Adding a stirring magneton (the rotating speed of the stirring magneton is 500 rmp) into the hydrothermal reaction kettle, and placing the hydrothermal reaction kettle in an oil bath kettle at the temperature of 140 ℃ for stirring reaction for 10 hours. And taking out the mixture after the reaction is finished, cooling the mixture, washing the mixture by using deionized water and ethanol until the washing liquid is neutral, and drying the washing liquid. The nitrogen-doped titanium dioxide photocatalysis self-cleaning agent is obtained, and the particle size of the nitrogen-doped titanium dioxide photocatalysis self-cleaning agent is 500 nm.
A preparation method of the nitrogen-doped titanium dioxide self-cleaning aqueous polyurethane coating comprises the following steps: the preparation method comprises the steps of ultrasonically dispersing nitrogen-doped titanium dioxide photocatalytic self-cleaning agent powder in deionized water for 30min, adding deionized water into a polyurethane prepolymer before emulsification in the preparation process of an aqueous polyurethane emulsion, slowly dripping the dispersion liquid into a reaction system, stirring until the mixture is uniformly mixed, emulsifying, distilling under reduced pressure to remove acetone to obtain a compound of polyurethane resin and the nitrogen-doped titanium dioxide photocatalytic self-cleaning agent powder, uniformly mixing a dispersing agent, a curing agent, a defoaming agent, a film-forming aid and a flatting agent in proportion, and uniformly mixing by utilizing a mechanical shearing action.
Example 2
The nitrogen-doped titanium dioxide self-cleaning waterborne polyurethane coating comprises the following raw materials in parts by weight: 35 parts of water, 60 parts of polyurethane resin, 0.4 part of nitrogen-doped titanium dioxide photocatalytic self-cleaning agent, 1.8 parts of dispersing agent, 1.3 parts of curing agent, 1 part of defoaming agent, 0.7 part of film-forming assistant and 0.8 part of flatting agent.
The dispersing agent is a carboxylic acid copolymer salt dispersing agent, the curing agent is a polyamide curing agent, the defoaming agent is an organic silicon defoaming agent, the film-forming assistant is an alcohol ether film-forming assistant, and the flatting agent is a polysiloxane flatting agent.
The preparation method of the nitrogen-doped titanium dioxide photocatalytic self-cleaning agent is the same as that of example 1.
A preparation method of the nitrogen-doped titanium dioxide self-cleaning aqueous polyurethane coating comprises the following steps: the preparation method comprises the steps of ultrasonically dispersing nitrogen-doped titanium dioxide photocatalytic self-cleaning agent powder in deionized water for 30min, adding deionized water into a polyurethane prepolymer before emulsification in the preparation process of an aqueous polyurethane emulsion, slowly dripping the dispersion liquid into a reaction system, stirring until the mixture is uniformly mixed, emulsifying, distilling under reduced pressure to remove acetone to obtain a compound of polyurethane resin and the nitrogen-doped titanium dioxide photocatalytic self-cleaning agent powder, uniformly mixing a dispersing agent, a curing agent, a defoaming agent, a film-forming aid and a flatting agent in proportion, and uniformly mixing by utilizing a mechanical shearing action.
Comparative example 1
The titanium dioxide antibacterial coating prepared under the ordinary hydrothermal condition comprises the following raw materials in parts by weight: 25 parts of water, 30 parts of acrylic resin, 20 parts of polyurethane resin, 0.5 part of titanium dioxide photocatalytic self-cleaning agent, 2.5 parts of dispersing agent, 1 part of curing agent, 0.8 part of defoaming agent, 0.8 part of film-forming assistant and 0.8 part of flatting agent.
After water, acrylic resin, polyurethane resin, a dispersing agent, a curing agent, a defoaming agent, a film-forming assistant and a flatting agent are uniformly mixed according to a proportion, a titanium dioxide photocatalytic self-cleaning agent is added into the mixture, and then the mixture is uniformly mixed by utilizing the mechanical shearing action to obtain the common titanium dioxide antibacterial coating.
Performance testing
1. Degradation rate of different materials to methylene blue
FIG. 1 shows the degradation rates of different materials for methylene blue, which are respectively a water-based polyurethane coating film, nitrogen-doped titanium dioxide powder, and N-TiO2a/WPU coating film. From the figure we can see pure WPU coating filmsHas little capability of degrading methylene blue when N-TiO is added2Then has the capability of degrading methylene blue.
2. Contact angle analysis of coating films with different nitrogen-doped titanium dioxide contents
FIG. 4 shows different N-TiO compounds2The contact angle between the WPU self-cleaning coating film and oleic acid is shown in the figure, wherein (a) is N-TiO-free2The contact angle of the aqueous polyurethane coating film with oleic acid was 90.4 °. (b) N-TiO in (c) and (d)2The addition amounts of (A) and (B) were 0.3%, 0.4% and 1.0%, respectively, and the contact angles with oleic acid were 64.3 °, 43.1 ° and 43.7 °, respectively. Under the irradiation of light, part of the oleic acid solution is dripped by the N-TiO2Catalytic degradation, which accounts for N-TiO2The addition of (2) does give the polyurethane film a self-cleaning property. And with N-TiO2The contact angle between the film layer and oleic acid did not decrease all the time as the addition amount increased, and the contact angle of the film added at 0.4% was about 43 ° as compared with that of the film added at 1%. Therefore, it was found that the photocatalytic efficiency reached the saturation state already at the addition level of 0.4%, and that 0.4% was N-TiO because the contact angle of the coating film at the addition level of 0.3% was 64.3 ℃ and larger than 43.1 °2The optimum amount of addition of (c).
TABLE 1 self-cleaning coating photocatalytic Performance Table
From the above table, it can be seen that the nitrogen-doped titanium dioxide self-cleaning aqueous polyurethane coating of the present invention has longer self-cleaning ability than the common self-cleaning coating and still has self-cleaning ability under white light.
TABLE 2 test of conventional Properties of Nitrogen-doped titanium dioxide self-cleaning waterborne polyurethane coating of the present invention
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (5)
1. The nitrogen-doped titanium dioxide self-cleaning waterborne polyurethane coating is characterized by comprising the following raw materials, by weight, 25 ~ 35 parts of water, 50 ~ 60 parts of polyurethane resin, 0.3 ~ 1.0.0 part of nitrogen-doped titanium dioxide photocatalytic self-cleaning agent, 1.5 ~ 2.5.5 parts of dispersing agent, 1 ~ 1.5.5 parts of curing agent, 0.8 ~ 1 part of defoaming agent, 0.5 ~ 0.8.8 part of film-forming assistant and 0.5 ~ 0.8.8 part of leveling agent;
the preparation method of the nitrogen-doped titanium dioxide photocatalytic self-cleaning agent comprises the following steps: adding TiN powder and concentrated sulfuric acid into a hydrothermal reaction kettle, adding stirring magnetons into the hydrothermal reaction kettle, placing the hydrothermal reaction kettle in an oil bath kettle at a certain temperature for stirring reaction, taking out the hydrothermal reaction kettle after a certain time, cooling the hydrothermal reaction kettle, washing the hydrothermal reaction kettle with deionized water and ethanol until a washing solution is neutral, and drying the washing solution to obtain the nitrogen-doped titanium dioxide photocatalytic self-cleaning agent;
the preparation method of the nitrogen-doped titanium dioxide self-cleaning waterborne polyurethane coating comprises the following steps: the preparation method comprises the steps of ultrasonically dispersing nitrogen-doped titanium dioxide photocatalytic self-cleaning agent powder in deionized water for 30min, adding deionized water into a polyurethane prepolymer before emulsification in the preparation process of an aqueous polyurethane emulsion, slowly dripping the dispersion liquid into a reaction system, stirring until the mixture is uniformly mixed, emulsifying, distilling under reduced pressure to remove acetone to obtain a compound of polyurethane resin and the nitrogen-doped titanium dioxide photocatalytic self-cleaning agent powder, uniformly mixing a dispersing agent, a curing agent, a defoaming agent, a film-forming aid and a flatting agent in proportion, and uniformly mixing by utilizing a mechanical shearing action.
2. The nitrogen-doped titanium dioxide self-cleaning aqueous polyurethane coating as claimed in claim 1, wherein the concentration of concentrated sulfuric acid is 5.0 mol/L, and the adding ratio of TiN powder and concentrated sulfuric acid is 1: 60 ~ 70 g/mL.
3. The nitrogen-doped titanium dioxide self-cleaning aqueous polyurethane coating according to claim 1, wherein the temperature of the hydrothermal reaction is 140 ℃ and the reaction time is 10 ~ 16 h.
4. The nitrogen-doped titanium dioxide self-cleaning aqueous polyurethane coating as claimed in claim 1, wherein the rotation speed of the stirring magnetons is 400 ~ 600 rmp.
5. The nitrogen-doped titanium dioxide self-cleaning aqueous polyurethane coating material as claimed in claim 1, wherein the particle size of the prepared nitrogen-doped titanium dioxide photocatalytic self-cleaning agent is 400 ~ 600 nm.
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| CN103992733A (en) * | 2014-06-13 | 2014-08-20 | 福州大学 | Water-borne wood paint with disinfecting, bacterial-resisting, VOC (Volatile Organic Compounds)-removing and purifying functions |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103992733A (en) * | 2014-06-13 | 2014-08-20 | 福州大学 | Water-borne wood paint with disinfecting, bacterial-resisting, VOC (Volatile Organic Compounds)-removing and purifying functions |
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