CN111087835A - Preparation method of nano self-cleaning environment-friendly coating - Google Patents
Preparation method of nano self-cleaning environment-friendly coating Download PDFInfo
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- CN111087835A CN111087835A CN201911211803.0A CN201911211803A CN111087835A CN 111087835 A CN111087835 A CN 111087835A CN 201911211803 A CN201911211803 A CN 201911211803A CN 111087835 A CN111087835 A CN 111087835A
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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
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C19/00—Other disintegrating devices or methods
- B02C19/20—Disintegrating by grating
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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
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/004—Reflecting paints; Signal paints
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- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/16—Antifouling paints; Underwater paints
- C09D5/1687—Use of special additives
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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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/32—Radiation-absorbing paints
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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
- C09D7/20—Diluents or solvents
Abstract
The invention discloses a preparation method of a nano self-cleaning environment-friendly coating, which comprises the steps of putting a nano titanium dioxide colloid into a stirring reaction kettle, adding deionized water, ethanol and an organic solvent for reaction to prepare a nano titanium dioxide colloid solution, adding the nano titanium dioxide colloid solution into a heating stirrer, simultaneously adding zeolite, an inorganic environment-friendly filler, polyvinylpyrrolidone and sodium benzoate, stirring for reaction to prepare a nano titanium dioxide emulsion, adding the nano titanium dioxide emulsion into the stirring kettle, and adding a thickening agent and a defoaming agent to prepare the nano self-cleaning environment-friendly coating, wherein the nano self-cleaning environment-friendly coating has super-hydrophobic and oleophobic properties and excellent self-cleaning properties; the invention also provides a ball milling device, which is used for grinding and refining titanium dioxide particles, the mixed materials roll and are ground and refined in the wheel sand cutting grooves arranged in the ball milling device, and the ball milling effect is good.
Description
Technical Field
The invention relates to the technical field of paint preparation, in particular to a preparation method of a nano self-cleaning environment-friendly paint.
Background
The nano environment-friendly coating is a product formed by butt-jointing nano materials and coatings, belongs to a high-tech functional coating, particularly relates to a coating which is prepared by a nano material preparation method such as a sol-gel method and the like and is completely composed of nano materials with the particle size of less than 100 nanometers, and is widely applied to the aspects of house wall painting, vehicle spraying and the like.
The self-cleaning coating can be used on the surface of a substrate (such as glass ceramic or wood stone and the like), and can play a role in preventing fouling and self cleaning by virtue of the hydrophobic or hydrophilic physical characteristics of the coating, the particle size of the coating enters a nanometer scale, the reaction capacity of chemical catalysis and photocatalysis can be improved by increasing the active center of the surface of the material, and the self-cleaning capability is provided for the coating under the action of ultraviolet rays and oxygen; the surface of the high-surface-energy nano material can obtain the characteristics of hydrophobicity and oleophobicity at the same time through modification, and the anti-fouling performance of the coating can be obviously improved and the weather resistance can be improved when the coating is used for the inner and outer wall coatings; the scrub resistance of the coating can be improved by adding the nano silicon dioxide into the outer wall coating; the nano titanium dioxide is added into the building exterior wall coating, so that the weather resistance of the emulsion paint can be improved to a new level, and the aging resistance of the emulsion paint is greatly improved.
However, the existing nano environment-friendly coating has poor self-cleaning performance, is coated on the surface of an object, and is easy to enrich organic matters such as water, grease and the like on the surface of the object after a period of time, so that the attractiveness of the coating is influenced, and meanwhile, the object is corroded and corroded by corrosion.
Disclosure of Invention
The invention aims to provide a preparation method of a nano self-cleaning environment-friendly coating.
The technical problems to be solved by the invention are as follows:
1. the environment-friendly coating produced by the prior art is easy to generate leveling and cracking phenomena in the using process, and the service life of the coating is shorter due to lower wear resistance and durability.
2. The environment-friendly coating produced by the prior art is coated on the surface of a workpiece, the surface of the workpiece is easy to rust, and after a period of time, moisture and organic pollutants are easy to adhere to the surface of the workpiece, so that the attractiveness of the workpiece is influenced, and the self-cleaning performance is poor.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of a nano self-cleaning environment-friendly coating comprises the following steps:
step one, taking 30-45 parts of nano titanium dioxide colloid in parts by weight, putting into a stirring reaction kettle, adding 50-60 parts of deionized water into the stirring reaction kettle, wherein the rotating speed of the stirring reaction kettle is 280 plus materials at 350r/min, heating to 80 ℃ at the heating rate of 5-7 ℃/min, stirring for 5-10min, preliminarily dispersing the nano titanium dioxide colloid into the deionized water, dropwise adding 5-10 parts of ethanol and 5-10 parts of organic solvent into the stirring reaction kettle, and setting the stirring time to be 20-30min, further dissolving the nano titanium dioxide colloid under the action of the ethanol and the organic solvent to obtain nano titanium dioxide colloid solution;
weighing 5-10 parts of zeolite, crushing to obtain zeolite powder with the particle size of 30-40nm, adding the nano titanium dioxide colloidal solution obtained in the step one into a heating stirrer, setting the rotation speed to be 200 plus materials at 300r/min, setting the temperature to be 90-95 ℃, firstly adding the ground zeolite powder into the heating stirrer, stirring for 5-10min, then adding 20-30 parts of inorganic environment-friendly filler, 15-20 parts of polyvinylpyrrolidone and 15-20 parts of sodium benzoate into the heating stirrer, and continuously stirring and reacting for 30-50min to obtain nano titanium dioxide emulsion;
and step three, placing the nano titanium dioxide colloidal solution obtained in the step one into a stirring kettle, setting the rotating speed to be 200-80 ℃ and the stirring temperature to be 70-80 ℃, firstly adding 3-5 parts of thickening agent into the stirring kettle, stirring for 5min, then adding 3-5 parts of defoaming agent into the stirring kettle, continuing stirring for 20-30min, and cooling to obtain the nano self-cleaning environment-friendly coating.
Wherein, the organic solvent added in the step one is any one of styrene, perchloroethylene or ethylene glycol ether;
the inorganic environment-friendly filler added in the second step is any one of calcium carbonate, kaolin or bentonite;
the defoaming agent added in the third step is any one of emulsified silicone oil or polydimethylsiloxane;
the thickener added in the third step is any one of gelatin or polyvinylpyrrolidone.
As a further scheme of the invention, the nano titanium dioxide colloid is prepared by the following steps:
1) adding 40-50 parts of titanium dioxide particles and 5-10 parts of zirconia ceramic microspheres into a grinding space of a ball milling device through a feeding port in parts by weight, ball milling by adopting a three-stage type speed-selecting dry method, opening an oil cylinder, driving a piston rod to move through the oil cylinder, simultaneously opening a rotating motor, driving a ball milling rod fixedly connected with an output shaft of the rotating motor to rotate through the rotating motor, further leading a grinding round head to rotate and push to move, further leading materials to rotate through a spiral wheel sand cutting groove arranged on the grinding round head, rolling continuously in the wheel sand cutting groove, grinding and refining, and obtaining mixture particles after ball milling by the three-stage speed-selecting dry method, wherein the particle size of nano titanium dioxide is 20-30nm;
2) leaching and filtering the mixture particles obtained in the step 1), removing the zirconia ceramic microspheres in the mixture particles to obtain a solution only containing the titania particles, putting the solution into a stirring reaction kettle, adding 3-5 parts of an emulsifier into the stirring reaction kettle, wherein the rotating speed of the stirring reaction kettle is 300-400r/min, the reaction temperature is 100-120 ℃, and the stirring time is 30-40min to obtain nano titania filaments;
3) adding the nano titanium dioxide filament obtained in the step 2) into a muffle furnace, heating to 120 ℃ at a heating rate of 5-7 ℃/min, keeping the temperature of 120 ℃ for burning the nano titanium dioxide filament for 30-50min, removing water in the nano titanium dioxide filament to obtain a preliminarily dried nano titanium dioxide colloid, putting the preliminarily dried nano titanium dioxide colloid into a drying oven, setting the drying temperature to be 110 ℃, and drying for 60-80min to obtain the nano titanium dioxide colloid;
wherein, the titanium dioxide particles selected in the step 1) are rutile type titanium dioxide, and the emulsifier in the step 2) is aqueous polyurethane emulsion.
As a further scheme of the invention, the ball milling method of the three-section type speed-selecting dry method in the step 1) comprises the following specific processes: the first stage is low-speed pre-ball milling, the rotating speed of a rotating motor is set to be 200-; the second stage is high-speed ball milling, the rotating speed of a rotating motor is set to be 500-600r/min, and the time is 5 min; the third stage is ball milling, the rotating speed of a rotating motor is set to be 200-300r/min, and the time is 5 min.
As a further scheme of the invention, the invention also provides a ball milling device, which comprises a ball milling chamber body, wherein the upper side wall of the ball milling chamber body is provided with a feed inlet, the lower side wall of the ball milling chamber body is provided with a discharge outlet, two ends of the side wall of the ball milling chamber body are respectively provided with a support seat, and the support seats are arranged for fixing the ball milling chamber body; the inner side surface of the left end of the ball milling chamber body is provided with an oil cylinder, the oil cylinder is fixedly connected with a piston rod, the other end of the piston rod is provided with a rotating motor, an output shaft of the rotating motor is fixedly connected with a ball milling rod, the other end of the ball milling rod is fixedly connected with a crushing round head, the side wall of the crushing round head is provided with a spiral wheel sand cutting groove, materials enter the wheel sand cutting groove of the crushing round head from a charging hole, the ball milling rod fixedly connected with the output shaft of the rotating motor is driven to rotate through the rotating motor, the crushing round head is further rotated, and the top of;
a sealing bearing is arranged in the side wall of the ball milling chamber body at the left end of the ball milling rod, the outer ring of the sealing bearing is fixedly connected with the side wall of the ball milling chamber body, the inner ring of the sealing bearing is fixedly connected with the ball milling rod, the arrangement of the sealing bearing prevents materials from leaking, and the investment of production cost is reduced;
be provided with on the right-hand member medial surface of ball-milling chamber body with smash button head complex round platform recess, be equipped with a plurality of protruding friction points on the round platform recess inside wall, protruding friction point is used for increasing the frictional force of material and round platform recess inside wall, further improves the material and refines the degree, improves ball-milling efficiency, smashes the outside of button head and forms the grinding space with the inboard of round platform recess.
The invention has the beneficial effects that:
1. according to the preparation method of the nano self-cleaning environment-friendly coating, when the environment-friendly coating is prepared, ethanol and organic solvent ethylene glycol ether are added into a stirring reaction kettle, so that a nano titanium dioxide colloid substance can be dissolved in a solution and is matched with the ethanol for use, and the dissolving effect is good; inorganic environment-friendly filler kaolin is added in the preparation process of the nano titanium dioxide emulsion, so that the rheological property of the coating is adjusted, the wear resistance and durability of the coating are improved, and the service life of the coating is prolonged; the emulsified silicone oil added in the step three is rapidly spread on the surface of the bubble after contacting with the bubble generated in the reaction process, and the emulsified silicone oil molecules are attached to the surface of the bubble film to reduce the local surface tension of the surface of the bubble film, so that the whole bubble can generate unbalanced stress to cause bubble breakage, and the defoaming effect is good; the polyvinylpyrrolidone added in the third step increases the viscosity of the coating, prevents the coating from leveling and cracking in the using process, and prolongs the service life.
2. According to the preparation method of the nano self-cleaning environment-friendly coating, when the nano titanium dioxide colloid is prepared, rutile titanium dioxide is selected, the rutile titanium dioxide has super-hydrophilicity, water drops are not easily formed on the surface of the rutile titanium dioxide, and organic pollutants adsorbed on the surface of the coating can be decomposed into carbon dioxide and oxygen, so that the self-cleaning function is realized, meanwhile, the nano titanium dioxide also has high refractivity and high optical activity, can reflect and scatter ultraviolet rays, can absorb the ultraviolet rays, has stronger barrier capability on the ultraviolet rays, and can improve the aging resistance of the coating when being used in the coating.
3. In order to better prepare the nano titanium dioxide colloid, the invention also provides a ball milling device which comprises a ball milling chamber body, wherein two ends of the side wall of the ball milling chamber body are respectively provided with a supporting seat for fixing the ball milling chamber body, the inner side surface of the left end of the ball milling chamber body is provided with an oil cylinder, the oil cylinder is fixedly connected with a piston rod, the other end of the piston rod is provided with a rotating motor, an output shaft of the rotating motor is fixedly connected with a ball milling rod, and the other end of the ball milling rod is fixedly connected with a crushing round head; the side wall of the grinding round head is provided with a spiral wheel sand cutting groove, materials enter the wheel sand cutting groove of the grinding round head from a charging opening, a ball milling rod fixedly connected with an output shaft of a rotating motor is driven to rotate through the rotating motor, the grinding round head is further rotated, the materials continuously roll in the wheel sand cutting groove, and the materials are ground and refined; the top of the crushing round head is provided with a wear-resistant pad, and the wear-resistant pad is used for preventing the inner side wall of the circular truncated cone groove from being rubbed when the top of the crushing round head contacts the circular truncated cone groove, so that the circular truncated cone groove is damaged, and the service life of the ball milling device is shortened; a sealing bearing is arranged in the side wall of the ball milling chamber body at the left end of the ball milling rod, the outer ring of the sealing bearing is fixedly connected with the side wall of the ball milling chamber body, the inner ring of the sealing bearing is fixedly connected with the ball milling rod, the arrangement of the sealing bearing prevents materials from leaking, and the investment of production cost is reduced; a round platform groove matched with the crushing round head is formed in the inner side face of the right end of the ball milling chamber body, a plurality of protruding friction points are arranged on the inner side wall of the round platform groove, and the protruding friction points are used for increasing the friction force between materials and the inner side wall of the round platform groove, so that the material refining degree is further improved, and the ball milling efficiency is improved; the outer side of the smashing round head and the inner side of the round platform groove form a grinding space, and the ball milling device is simple in structure, good in grinding effect and practical.
Drawings
The invention will be further described with reference to the accompanying drawings.
FIG. 1 is a schematic sectional view of a ball milling apparatus according to the present invention;
FIG. 2 is a schematic side view of a ball milling apparatus of the present invention;
fig. 3 is a schematic view of the structure of the pulverization button head.
In the figure: 1. a ball milling chamber body; 11. a feed inlet; 12. a discharge port; 13. sealing the bearing; 2. an oil cylinder; 21. a piston rod; 22 a rotating electrical machine; 3. a ball milling rod; 4. smashing round heads; 41. cutting grooves in wheel sand; 42. a wear pad; 5. a circular truncated cone groove; 6. a milling space; 7. and (4) supporting the base.
Detailed Description
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 only a part of the embodiments of the present invention, and not all of the 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 preparation method of a nano self-cleaning environment-friendly coating comprises the following steps:
step one, 40 parts by weight of nano titanium dioxide colloid is placed into a stirring reaction kettle, 55 parts by weight of deionized water is added into the stirring reaction kettle, the rotating speed of the stirring reaction kettle is 320r/min, the temperature is increased to 80 ℃ at the heating rate of 6 ℃/min, after stirring for 8min, the nano titanium dioxide colloid is primarily dispersed into the deionized water, 8 parts by weight of ethanol and 8 parts by weight of organic solvent are dropwise added into the stirring reaction kettle, the stirring time is set to 25min, and the nano titanium dioxide colloid is further dissolved under the action of the ethanol and the organic solvent to obtain nano titanium dioxide colloid solution;
weighing 8 parts of zeolite, crushing to obtain zeolite powder with the particle size of 30-40nm, adding the nano titanium dioxide colloidal solution obtained in the step one into a heating stirrer, setting the rotating speed to be 250r/min and the temperature to be 92 ℃, firstly adding the ground zeolite powder into the heating stirrer, stirring for 7min, then adding 25 parts of inorganic environment-friendly filler, 18 parts of polyvinylpyrrolidone and 18 parts of sodium benzoate into the heating stirrer, and continuously stirring and reacting for 40min to obtain nano titanium dioxide emulsion;
and step three, putting the nano titanium dioxide colloidal solution obtained in the step one into a stirring kettle, setting the rotating speed to be 260r/min and the stirring temperature to be 75 ℃, firstly adding 4 parts of thickening agent into the stirring kettle, stirring for 5min, then adding 4 parts of defoaming agent into the stirring kettle, continuously stirring for 25min, and cooling to obtain the nano self-cleaning environment-friendly coating.
The organic solvent added in the step one is ethylene glycol ether, and the nano titanium dioxide colloid can be dissolved in the solution by adding the organic solvent ethylene glycol ether, and the organic solvent ethylene glycol ether is matched with ethanol for use, so that the dissolving effect is good;
the inorganic environment-friendly filler added in the second step is kaolin, and the addition of the kaolin can adjust the rheological property of the coating, improve the wear resistance and durability of the coating and prolong the service life of the coating;
the defoaming agent added in the third step is emulsified silicone oil, a large number of bubbles are easily generated in the production process of the coating, if the influence on the finished product quality of the coating is not eliminated in time, the added emulsified silicone oil is quickly spread on the surface of the bubbles after contacting the bubbles, the surface tension of the emulsified silicone oil is lower than that of the bubble liquid, and the emulsified silicone oil molecules are attached to the surface of the bubble film to reduce the local surface tension of the surface of the bubble film and keep larger surface tension on the rest part of the film surface, so that the whole bubbles can generate unbalanced stress to cause bubble breakage, and the defoaming effect is good;
the thickening agent added in the third step is polyvinylpyrrolidone, and the addition of the polyvinylpyrrolidone increases the viscosity of the coating, prevents the coating from leveling and cracking in the use process, and prolongs the service life.
Wherein, the nanometer titanium dioxide colloid in the step one is prepared by the following steps:
1) adding 45 parts of titanium dioxide particles and 8 parts of zirconia ceramic microspheres into a grinding space 6 of a ball milling device through a feeding port 11 by weight parts, performing ball milling by adopting a three-stage type speed-selecting dry method, opening an oil cylinder 2, driving a piston rod 21 to move through the oil cylinder 2, simultaneously opening a rotating motor 22, driving a ball milling rod 3 fixedly connected with an output shaft of the rotating motor 22 to rotate through the rotating motor 22, further enabling a grinding round head 4 to rotate and move in a rotary propulsion manner, further rotating through a spiral wheel sand cutting groove 41 arranged on the grinding round head 4, continuously rolling and refining materials in the wheel sand cutting groove 41, and grinding the mixture particles obtained after ball milling by the three-stage speed-selecting dry method to obtain nano titanium dioxide particles with the particle size of 20-30nm;
2) leaching and filtering the mixture particles obtained in the step 1), removing zirconia ceramic microspheres in the mixture particles to obtain a solution only containing titanium dioxide particles, putting the solution into a stirring reaction kettle, adding 4 parts of emulsifier into the stirring reaction kettle, setting the rotating speed of the stirring reaction kettle to be 350r/min, setting the reaction temperature to be 110 ℃, and stirring for 35min to obtain nano titanium dioxide filaments;
3) adding the nano titanium dioxide filament obtained in the step 2) into a muffle furnace, heating to 120 ℃ at a heating rate of 6 ℃/min, keeping the temperature of 120 ℃ for burning the nano titanium dioxide filament for 40min, removing water in the nano titanium dioxide filament to obtain a preliminarily dried nano titanium dioxide colloid, putting the preliminarily dried nano titanium dioxide colloid into an oven, setting the drying temperature to be 110 ℃, and drying for 70min to obtain the nano titanium dioxide colloid.
The ball milling method of the three-section type speed-selecting dry method in the step 1) comprises the following specific processes:
the first stage is low-speed pre-ball milling, the rotating speed of the rotating motor 22 is set to be 250r/min, the time is 5min, the low-speed pre-ball milling is set to prevent the titanium dioxide particles from being uneven in size, and the service life of the ball mill is reduced by directly carrying out high-speed ball milling in the ball mill;
the second stage is high-speed ball milling, the rotating speed of the rotating motor 22 is set to be 550r/min, the time is 5min, and the high-speed ball milling is set to quickly crush the titanium dioxide particles subjected to ball milling into particles with smaller particle size;
the third stage is post ball milling, the rotating speed of the rotating motor 22 is set to be 250r/min, the time is 5min, the post ball milling is set to further break and refine titanium dioxide particles, and the particle size of the obtained mixture particles is 20-40 nm.
The titanium dioxide particles selected in the step 1) are rutile type titanium dioxide, and the rutile type titanium dioxide has higher hardness, density, dielectric constant and refractive index, higher thermal stability and super-hydrophilicity, the surface of the coating is not easy to form water drops, the nano titanium dioxide is added into the coating to produce the antibacterial and antifouling coating with sterilization, antifouling and self-cleaning functions, the titanium dioxide is activated and generates free radicals with high catalytic activity under the action of ultraviolet rays, the high photooxidation and reduction capability can be generated, organic pollutants adsorbed on the surface of the coating can be decomposed into carbon dioxide and oxygen, the nano titanium dioxide has high refractivity and high photoactivity, small particle size and high activity, can reflect and scatter ultraviolet rays and absorb ultraviolet rays, has stronger barrier capability on the ultraviolet rays, and can improve the aging resistance of the coating when being used in the coating;
the zirconia ceramic microspheres added in the step 1) have good roundness, smooth surface, impact resistance, low abrasion and good toughness, do not crack or peel in a high-speed and high-concentration machine, are added into a ball milling device as a grinding medium, have high grinding efficiency and are beneficial to the crushing and refining of titanium dioxide particles;
the emulsifier in the step 2) is aqueous polyurethane emulsion which can improve the surface tension among various constituent phases in the solution to form uniform and stable emulsion substances, and the molecules of the aqueous polyurethane emulsion simultaneously have hydrophilic groups and hydrophilic oil groups which are gathered on an oil/water interface, so that the interfacial tension can be reduced, the energy required for forming the emulsion can be reduced, the surface tension of the liquid and the solid can be reduced, the liquid can be rapidly diffused to the whole surface, and the formation of nano titanium dioxide filaments is facilitated.
Example 2
A preparation method of a nano self-cleaning environment-friendly coating comprises the following steps:
step one, putting 30 parts of nano titanium dioxide colloid into a stirring reaction kettle, adding 50 parts of deionized water into the stirring reaction kettle, wherein the rotating speed of the stirring reaction kettle is 280r/min, heating to 80 ℃ at the heating rate of 5 ℃/min, stirring for 5min, preliminarily dispersing the nano titanium dioxide colloid into the deionized water, dropwise adding 5 parts of ethanol and 5 parts of organic solvent into the stirring reaction kettle, setting the stirring time to be 20min, and further dissolving the nano titanium dioxide colloid under the action of the ethanol and the organic solvent to obtain nano titanium dioxide colloid solution;
weighing 10 parts of zeolite, crushing to obtain zeolite powder with the particle size of 30-40nm, adding the nano titanium dioxide colloidal solution obtained in the step one into a heating stirrer, setting the rotating speed at 300r/min and the temperature at 95 ℃, firstly adding the ground zeolite powder into the heating stirrer, stirring for 10min, then adding 30 parts of inorganic environment-friendly filler, 20 parts of polyvinylpyrrolidone and 20 parts of sodium benzoate into the heating stirrer, and continuously stirring and reacting for 50min to obtain nano titanium dioxide emulsion;
step three, putting the nano titanium dioxide colloidal solution obtained in the step one into a stirring kettle, setting the rotating speed to be 300r/min, setting the stirring temperature to be 70 ℃, firstly adding 3 parts of thickening agent into the stirring kettle, stirring for 5min, then adding 3 parts of defoaming agent into the stirring kettle, continuing stirring for 20min, and cooling to obtain the nano self-cleaning environment-friendly coating;
the organic solvent added in the first step is styrene;
the inorganic environment-friendly filler added in the second step is calcium carbonate;
the defoaming agent added in the third step is polydimethylsiloxane;
the thickener added in the third step is gelatin.
Wherein, the nanometer titanium dioxide colloid in the step one is prepared by the following steps:
1) adding 40 parts of titanium dioxide particles and 5 parts of zirconia ceramic microspheres into a grinding space 6 of a ball milling device through a feeding port 11 by weight parts, performing ball milling by adopting a three-stage type speed-selecting dry method, opening an oil cylinder 2, driving a piston rod 21 to move through the oil cylinder 2, simultaneously opening a rotating motor 22, driving a ball milling rod 3 fixedly connected with an output shaft of the rotating motor 22 to rotate through the rotating motor 22, further enabling a grinding round head 4 to rotate and move in a rotary propulsion manner, further rotating through a spiral wheel sand cutting groove 41 arranged on the grinding round head 4, continuously rolling and refining materials in the wheel sand cutting groove 41, and grinding the mixture particles obtained after ball milling by the three-stage speed-selecting dry method to obtain nano titanium dioxide particles with the particle size of 20-30nm;
2) leaching and filtering the mixture particles obtained in the step 1), removing zirconia ceramic microspheres in the mixture particles to obtain a solution only containing titanium dioxide particles, putting the solution into a stirring reaction kettle, adding 3 parts of emulsifier into the stirring reaction kettle, setting the rotating speed of the stirring reaction kettle at 300r/min, the reaction temperature at 120 ℃, and stirring for 30min to obtain nano titanium dioxide filaments;
3) adding the nano titanium dioxide filament obtained in the step 2) into a muffle furnace, heating to 120 ℃ at a heating rate of 5 ℃/min, keeping the temperature of 120 ℃ for burning the nano titanium dioxide filament for 30min, removing water in the nano titanium dioxide filament to obtain a preliminarily dried nano titanium dioxide colloid, putting the preliminarily dried nano titanium dioxide colloid into an oven, setting the drying temperature to be 110 ℃, and drying for 60min to obtain the nano titanium dioxide colloid.
The ball milling method of the three-section type speed-selecting dry method in the step 1) comprises the following specific processes:
the first stage is low-speed pre-ball milling, the rotating speed of the rotating motor 22 is set to be 200r/min, the time is 5min, the low-speed pre-ball milling is set to prevent the titanium dioxide particles from being uneven in size, and the service life of the ball mill is reduced by directly carrying out high-speed ball milling in the ball mill;
the second stage is high-speed ball milling, the rotating speed of the rotating motor 22 is set to be 500r/min, the time is 5min, and the high-speed ball milling is set to quickly crush the titanium dioxide particles subjected to ball milling into particles with smaller particle size;
the third stage is post ball milling, the rotating speed of the rotating motor 22 is set to be 300r/min, the time is 5min, the post ball milling is set to further break and refine titanium dioxide particles, and the particle size of the obtained mixture particles is 20-40 nm.
The titanium dioxide particles selected in the step 1) are rutile type titanium dioxide;
the emulsifier in the step 2) is aqueous polyurethane emulsion.
Example 3
A preparation method of a nano self-cleaning environment-friendly coating comprises the following steps:
step one, 45 parts by weight of nano titanium dioxide colloid is placed into a stirring reaction kettle, 60 parts by weight of deionized water is added into the stirring reaction kettle, the rotating speed of the stirring reaction kettle is 350r/min, the temperature is increased to 80 ℃ at the heating rate of 7 ℃/min, after stirring for 10min, the nano titanium dioxide colloid is preliminarily dispersed into the deionized water, 10 parts by weight of ethanol and 10 parts by weight of organic solvent are dropwise added into the stirring reaction kettle, the stirring time is set to 30min, and the nano titanium dioxide colloid is further dissolved under the action of the ethanol and the organic solvent to obtain nano titanium dioxide colloid solution;
weighing 5 parts of zeolite, crushing to obtain zeolite powder with the particle size of 30-40nm, adding the nano titanium dioxide colloidal solution obtained in the step one into a heating stirrer, setting the rotating speed at 200r/min and the temperature at 90 ℃, firstly adding the ground zeolite powder into the heating stirrer, stirring for 5min, then adding 20 parts of inorganic environment-friendly filler, 15 parts of polyvinylpyrrolidone and 15 parts of sodium benzoate into the heating stirrer, and continuously stirring and reacting for 30min to obtain nano titanium dioxide emulsion;
step three, putting the nano titanium dioxide colloidal solution obtained in the step one into a stirring kettle, setting the rotating speed to be 200r/min, setting the stirring temperature to be 80 ℃, firstly adding 5 parts of thickening agent into the stirring kettle, stirring for 5min, then adding 5 parts of defoaming agent into the stirring kettle, continuously stirring for 30min, and cooling to obtain the nano self-cleaning environment-friendly coating;
wherein the organic solvent added in the step one is perchloroethylene;
the inorganic environment-friendly filler added in the second step is kaolin;
the defoaming agent added in the third step is emulsified silicone oil;
the thickener added in the third step is gelatin.
Wherein, the nanometer titanium dioxide colloid in the step one is prepared by the following steps:
1) adding 40-50 parts of titanium dioxide particles and 5-10 parts of zirconia ceramic microspheres into a grinding space 6 of a ball milling device through a feeding port 11 in parts by weight, performing ball milling by adopting a three-stage speed-selecting dry method, opening an oil cylinder 2, driving a piston rod 21 to move through the oil cylinder 2, simultaneously opening a rotating motor 22, driving a ball milling rod 3 fixedly connected with an output shaft of the rotating motor 22 to rotate through the rotating motor 22, further enabling a grinding round head 4 to rotate and move in a propelling manner, further rotating through a spiral wheel sand cutting groove 41 arranged on the grinding round head 4, enabling materials to continuously roll in the wheel sand cutting groove 41, grinding and refining, and obtaining mixture particles after ball milling by the three-stage speed-selecting dry method, wherein the particle size of nano titanium dioxide is 20-30nm;
2) leaching and filtering the mixture particles obtained in the step 1), removing the zirconia ceramic microspheres in the mixture particles to obtain a solution only containing the titania particles, putting the solution into a stirring reaction kettle, adding 5 parts of an emulsifier into the stirring reaction kettle, setting the rotating speed of the stirring reaction kettle at 400r/min, the reaction temperature at 100 ℃ and the stirring time at 40min to obtain nano titania filaments;
3) adding the nano titanium dioxide filament obtained in the step 2) into a muffle furnace, heating to 120 ℃ at a heating rate of 7 ℃/min, keeping the temperature of 120 ℃ for burning the nano titanium dioxide filament for 50min, removing water in the nano titanium dioxide filament to obtain a preliminarily dried nano titanium dioxide colloid, putting the preliminarily dried nano titanium dioxide colloid into an oven, setting the drying temperature to be 110 ℃, and drying for 80min to obtain the nano titanium dioxide colloid.
The ball milling method of the three-section type speed-selecting dry method in the step 1) comprises the following specific processes:
the first stage is low-speed pre-ball milling, the rotating speed of a rotating motor 22 is set to be 300r/min, the time is 5min, the low-speed pre-ball milling is set to prevent titanium dioxide particles from being uneven in size, and the service life of the ball mill is shortened by directly carrying out high-speed ball milling in the ball mill;
the second stage is high-speed ball milling, the rotating speed of the rotating motor 22 is set to be 600r/min, the time is 5min, and the high-speed ball milling is set to quickly crush the titanium dioxide particles subjected to ball milling into particles with smaller particle size;
the third stage is post ball milling, the rotating speed of the rotating motor 22 is set to be 200r/min, the time is 5min, the post ball milling is set to further break and refine titanium dioxide particles, and the particle size of the obtained mixture particles is 20-40 nm.
The titanium dioxide particles selected in the step 1) are rutile type titanium dioxide;
the emulsifier in the step 2) is aqueous polyurethane emulsion.
Comparative example 1
A preparation method of a nano self-cleaning environment-friendly coating comprises the preparation method of example 1, wherein 40 parts of nano titanium dioxide colloid is changed into 40 parts of common nano titanium dioxide powder.
The following test experiments were carried out on the properties of the environment-friendly coatings prepared in example 1, example 2, example 3 and comparative example 1:
experiment one: the environment-friendly coatings prepared in example 1, example 2, example 3 and comparative example 1 were applied to the surfaces of the same workpieces, a drop of deionized water was dropped on each workpiece surface, each workpiece was placed in a contact angle measuring instrument, the contact angle of the drop of deionized water with the coating on the workpiece surface was measured directly by the contact angle measuring instrument, and the measured contact angle was recorded in table 1.
Experiment two: the environmental protection coatings prepared in example 1, example 2, example 3 and comparative example 1 were applied to the surfaces of the same workpieces, the same weight parts of the same organic pollutants were dropped on the coatings on the surfaces of the workpieces, the weights of the workpieces were recorded, the workpieces were placed in a storage chamber for 20 days, the workpieces were weighed again, the weights of the workpieces after being placed for 20 days were recorded, and the results are shown in table 1.
TABLE 1
| Performance testing of environmentally friendly coatings | Example 1 | Example 2 | Example 3 | Comparative example 1 |
| Contact Angle size (°) | 10 | 12 | 12 | 150 |
| Quality (g) of work 20 days before storage | 237 | 236 | 238 | 237 |
| Quality of work (g) after 20 days of storage | 220 | 220 | 223 | 236 |
| Mass change of work (indicated by "+", "-", g) | -17 | -16 | -15 | -1 |
From the first experiment and the table 1, it can be known that the environmental protection coatings prepared in the first embodiment, the second embodiment and the third embodiment all have nano titanium dioxide colloid, the nano titanium dioxide colloid in the environmental protection coating in the first embodiment is changed into common nano titanium dioxide powder, and the contact angle data recorded in the table 1 shows that the contact angle between the environmental protection coating added with the nano titanium dioxide colloid and deionized water is obviously smaller than that of the environmental protection coating without the nano titanium dioxide colloid, and the nano self-cleaning environmental protection coating prepared by the invention has higher super-hydrophilic performance;
from the second experiment and table 1, it can be seen that the environmental protection coatings prepared in examples 1, 2, 3 and 1 are respectively coated on the surfaces of the same workpieces, the same organic pollutants are respectively dropped on the coatings on the surfaces of the workpieces in the same weight parts, and after the coatings are respectively placed in a storage room for 20 days, the mass reduction amount of the workpieces in examples 1, 2 and 3 is obviously greater than that of the workpieces in comparative example 1, which indicates that the environmental protection coatings added with the nano titanium dioxide colloid decompose the organic pollutants adsorbed on the surfaces of the environmental protection coatings into carbon dioxide and oxygen, thereby realizing the self-cleaning function.
In conclusion, the nano self-cleaning environment-friendly coating prepared by the invention has better super-hydrophobic oleophobic property and shows good self-cleaning property.
Please refer to fig. 1-3: in the above embodiment, the ball milling device includes a ball milling chamber body 1, the ball milling chamber body 1 is a cylindrical structure, a charging port 11 is arranged on the upper side wall of the ball milling chamber body 1, a discharging port 12 is arranged on the lower side wall of the ball milling chamber body 1, two ends of the side wall of the ball milling chamber body 1 are respectively provided with a supporting seat 7, and the supporting seats 7 are arranged for fixing the ball milling chamber body 1;
an oil cylinder 2 is arranged on the inner side surface of the left end of the ball milling chamber body 1, the oil cylinder 2 is fixedly connected with a piston rod 21, the other end of the piston rod 21 is provided with a rotating motor 22, an output shaft of the rotating motor 22 is fixedly connected with a ball milling rod 3, and the other end of the ball milling rod 3 is fixedly connected with a crushing round head 4;
the grinding round head 4 is of a round table structure, spiral wheel sand cutting grooves 41 are formed in the side wall of the grinding round head 4, materials enter the wheel sand cutting grooves 41 of the grinding round head 4 from the feeding port 11, the rotary motor 22 drives the ball milling rod 3 fixedly connected with the output shaft of the rotary motor 22 to rotate, the grinding round head 4 is further rotated, and the materials continuously roll in the wheel sand cutting grooves 41 and are ground and refined;
the top of the crushing round head 4 is provided with a wear-resistant pad 42, and the wear-resistant pad 42 is used for preventing the top of the crushing round head 4 from rubbing the inner side wall of the circular truncated cone groove 5 when contacting the circular truncated cone groove 5, so that the circular truncated cone groove 5 is damaged, and the service life of the ball milling device is shortened;
a sealing bearing 13 is arranged in the side wall of the ball milling chamber body 1 at the left end of the ball milling rod 3, the outer ring of the sealing bearing 13 is fixedly connected with the side wall of the ball milling chamber body 1, the inner ring of the sealing bearing 13 is fixedly connected with the ball milling rod 3, the arrangement of the sealing bearing 13 prevents materials from leaking, and the investment of production cost is reduced;
a circular truncated cone groove 5 matched with the crushing round head 4 is formed in the inner side face of the right end of the ball milling chamber body 1, a plurality of protruding friction points are arranged on the inner side wall of the circular truncated cone groove 5, and the protruding friction points are used for increasing the friction force between materials and the inner side wall of the circular truncated cone groove 5, so that the material thinning degree is further improved, and the ball milling efficiency is improved;
the outer side of the crushing round head 4 and the inner side of the round platform groove 5 form a grinding space 6.
The working method of the ball milling device comprises the following steps: zirconia ceramic microspheres and titanium dioxide particles are added into a pre-grinding space 6 of a ball-milling device through a feeding port 11, an oil cylinder 2 is opened, a piston rod 21 is driven to move through the oil cylinder 2, a rotating motor 22 is simultaneously opened, a ball-milling rod 3 fixedly connected with an output shaft of the rotating motor 22 is driven to rotate through the rotating motor 22, then a grinding round head 4 is driven to move in a rotating and pushing manner, further a spiral wheel sand cutting groove 41 is formed in the side wall of the grinding round head 4 to rotate, and mixed materials continuously roll in the wheel sand cutting groove 41 and are ground and refined; after the ball milling is finished, the discharge port 12 is opened, the mixed material is discharged from the discharge port 12, and the ball milling effect is good.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (8)
1. A preparation method of a nano self-cleaning environment-friendly coating is characterized by comprising the following steps:
step one, taking 30-45 parts of nano titanium dioxide colloid in parts by weight, putting into a stirring reaction kettle, adding 50-60 parts of deionized water into the stirring reaction kettle, wherein the rotating speed of the stirring reaction kettle is 280 plus materials at 350r/min, heating to 80 ℃ at the heating rate of 5-7 ℃/min, stirring for 5-10min, preliminarily dispersing the nano titanium dioxide colloid into the deionized water, dropwise adding 5-10 parts of ethanol and 5-10 parts of organic solvent into the stirring reaction kettle, and setting the stirring time to be 20-30min, further dissolving the nano titanium dioxide colloid under the action of the ethanol and the organic solvent to obtain nano titanium dioxide colloid solution;
weighing 5-10 parts of zeolite, crushing to obtain zeolite powder with the particle size of 30-40nm, adding the nano titanium dioxide colloidal solution obtained in the step one into a heating stirrer at the rotation speed of 200-300r/min and the temperature of 90-95 ℃, adding the ground zeolite powder into the heating stirrer, stirring for 5-10min, adding 20-30 parts of inorganic environment-friendly filler, 15-20 parts of polyvinylpyrrolidone and 15-20 parts of sodium benzoate into the heating stirrer, and continuously stirring and reacting for 30-50min to obtain nano titanium dioxide emulsion;
and step three, putting the nano titanium dioxide emulsion obtained in the step two into a stirring kettle, setting the rotating speed to be 200-80 ℃ and the stirring temperature to be 70-80 ℃, firstly adding 3-5 parts of thickening agent into the stirring kettle, stirring for 5min, then adding 3-5 parts of defoaming agent into the stirring kettle, continuing stirring for 20-30min, and cooling to obtain the nano self-cleaning environment-friendly coating.
2. The method for preparing a nano self-cleaning environment-friendly coating according to claim 1, wherein the organic solvent added in the step one is any one of styrene, perchloroethylene or ethylene glycol ether, the inorganic environment-friendly filler added in the step two is any one of calcium carbonate, kaolin or bentonite, the defoaming agent added in the step three is any one of silicone emulsion or polydimethylsiloxane, and the thickening agent added in the step three is any one of gelatin or polyvinylpyrrolidone.
3. The method for preparing nano self-cleaning environment-friendly paint according to claim 1, wherein the nano titanium dioxide colloid is prepared by the following steps:
1) adding 40-50 parts of titanium dioxide particles and 5-10 parts of zirconia ceramic microspheres into a grinding space (6) of a ball milling device through a feeding port (11) in parts by weight, performing ball milling by adopting a three-stage speed-selecting dry method, opening an oil cylinder (2), driving a piston rod (21) to move through the oil cylinder (2), simultaneously opening a rotating motor (22), driving a ball milling rod (3) fixedly connected with an output shaft of the rotating motor (22) to rotate through the rotating motor (22), further enabling a grinding round head (4) to rotate and move in a pushing manner, further enabling materials to rotate through a spiral wheel sand cutting groove (41) arranged on the grinding round head (4), continuously rolling the materials in the wheel sand cutting groove (41), grinding and refining, and obtaining mixture particles after ball milling by the three-stage speed-selecting dry method, wherein the particle size of nano titanium dioxide is 20-30nm;
2) leaching and filtering the mixture particles obtained in the step 1), removing the zirconia ceramic microspheres in the mixture particles to obtain a solution only containing the titania particles, putting the solution into a stirring reaction kettle, adding 3-5 parts of an emulsifier into the stirring reaction kettle, wherein the rotating speed of the stirring reaction kettle is 300-400r/min, the reaction temperature is 100-120 ℃, and the stirring time is 30-40min to obtain nano titania filaments;
3) adding the nano titanium dioxide filament obtained in the step 2) into a muffle furnace, heating to 120 ℃ at a heating rate of 5-7 ℃/min, keeping the temperature of 120 ℃ for burning the nano titanium dioxide filament for 30-50min, removing water in the nano titanium dioxide filament to obtain a preliminarily dried nano titanium dioxide colloid, putting the preliminarily dried nano titanium dioxide colloid into a drying oven, setting the drying temperature to be 110 ℃, and drying for 60-80min to obtain the nano titanium dioxide colloid.
4. The method for preparing a nano self-cleaning environment-friendly coating according to claim 3, wherein the titanium dioxide particles selected in the step 1) are rutile type titanium dioxide, and the emulsifier in the step 2) is aqueous polyurethane emulsion.
5. The preparation method of the nano self-cleaning environment-friendly coating as claimed in claim 3, wherein the ball milling method by the three-stage type speed-selecting dry method in the step 1) comprises the following specific steps: the first stage is low-speed pre-ball milling, the rotating speed of a rotating motor (22) is set to be 200-300r/min, and the time is 5 min; the second stage is high-speed ball milling, the rotating speed of a rotating motor (22) is set to be 500-; the third stage is ball milling, the rotating speed of a rotating motor (22) is set to be 200-300r/min, and the time is 5 min.
6. The preparation method of the nano self-cleaning environment-friendly coating according to claim 3, characterized in that the ball milling device comprises a ball milling chamber body (1), the ball milling chamber body (1) is of a cylindrical structure, a feeding port (11) is arranged on the upper side wall of the ball milling chamber body (1), a discharging port (12) is arranged on the lower side wall of the ball milling chamber body (1), two ends of the side wall of the ball milling chamber body (1) are respectively provided with a supporting seat (7), and the supporting seats (7) are arranged for fixing the ball milling chamber body (1);
an oil cylinder (2) is arranged on the inner side face of the left end of the ball milling chamber body (1), the oil cylinder (2) is fixedly connected with a piston rod (21), the other end of the piston rod (21) is provided with a rotating motor (22), an output shaft of the rotating motor (22) is fixedly connected with a ball milling rod (3), and the other end of the ball milling rod (3) is fixedly connected with a crushing round head (4);
the crushing round head (4) is in a round table structure, and spiral wheel sand cutting grooves (41) are formed in the side wall of the crushing round head (4);
a sealing bearing (13) is arranged in the side wall of the ball milling chamber body (1) at the left end of the ball milling rod (3), the outer ring of the sealing bearing (13) is fixedly connected with the side wall of the ball milling chamber body (1), and the inner ring of the sealing bearing (13) is fixedly connected with the ball milling rod (3);
a round platform groove (5) matched with the crushing round head (4) is formed in the inner side face of the right end of the ball milling chamber body (1);
the outer side of the crushing round head (4) and the inner side of the round platform groove (5) form a grinding space (6).
7. The method for preparing nano self-cleaning environment-friendly paint as claimed in claim 6, wherein the top of the smashing round head (4) is provided with a wear pad (42).
8. The method for preparing nano self-cleaning environment-friendly paint as claimed in claim 6, wherein a plurality of protruding friction points are arranged on the inner side wall of the circular truncated cone groove (5).
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