CN115960531A - Preparation method of long-acting anti-sticking coating - Google Patents
Preparation method of long-acting anti-sticking coating Download PDFInfo
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/10—Greenhouse gas [GHG] capture, material saving, heat recovery or other energy efficient measures, e.g. motor control, characterised by manufacturing processes, e.g. for rolling metal or metal working
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Abstract
The invention provides a preparation method of a long-acting anti-sticking coating, which comprises the following steps: adding deionized water, thickener polyhydroxyethyl cellulose and perfluoropolyether diol into a closed reaction kettle, slowly stirring, heating, and adding rutile type nano TiO 2 Sanding, adding defoaming agent, stirring, uniformly stirring liquid, adding photosensitive chlorineStanding and cooling the polyamic acid emulsion, continuously adding a polyisocyanate prefabricated product, and adjusting the pH value of the liquid to obtain a product A; respectively adding fluorine-silicon modified polyester resin, a hydrophobic restoring agent and a mildew-proof and algae-proof agent, placing the mixture into a reaction kettle for soaking reaction for 2 hours, stirring, mixing and preserving heat, after cooling, dropwise adding secondary aminosilane into the reaction kettle, continuously introducing ammonia gas for reaction, and after dropwise adding is finished, standing to obtain a product B; and (3) putting the product A and the product B into a reaction kettle, adding a cross-linking agent and an organic solvent, fusing, filtering and discharging to obtain the long-acting anti-sticking coating.
Description
Technical Field
The application relates to the technical field of coatings, in particular to a preparation method of a long-acting anti-sticking coating.
Background
With the rapid development of economy and the increasing demand of people for information, various phenomena of messy advertisement pasting are emerging, and the small advertisements pasted on the surfaces of buildings are not easy to tear off, so that the urban psoriasis is extremely discordant. Because the urban small advertisements are firmly adhered to the surfaces of urban facilities, the residual small advertisements cannot be cleaned by the existing cleaning technology and cleaning agent, and patch-type pollution and turbid pollution left after cleaning are caused, so that the urban persistent ailment not only brings huge burden to sanitation workers, but also seriously affects the attractiveness of cities;
CN104356774B discloses an anti-doodling paint, which comprises the following components in parts by weight: 0.5 to 1.5 percent of dispersant, 0.1 to 0.3 percent of defoamer, 0.05 to 0.15 percent of wetting agent, 1 to 3 percent of film-forming additive, 20 to 35 percent of EVA emulsion, 9 to 29 percent of fluorosilicone resin, 1 to 12 percent of fluorine-containing nano-silica dispersion, 0.5 to 2 percent of coupling agent and 23 to 33.5 percent of pigment and filler;
the prior art has the following problems:
(1) The introduced auxiliary agent is more and has lower hardness, the surface becomes sticky along with the precipitation of the auxiliary agent caused by photo-oxidative aging, and the use aging is shorter;
(2) The anti-doodling paint is easy to fall off when meeting water, is limited in use occasions and is not suitable for outdoor occasions;
therefore, the invention provides a preparation method of a long-acting anti-sticking coating.
Disclosure of Invention
The application aims to provide a preparation method of a long-acting anti-sticking coating, and aims to solve the problems that the existing anti-doodling anti-sticking coating in the background art is low in hardness, short in use time effect and limited in application occasions.
In order to achieve the above purpose, the present application provides the following technical solutions:
the application provides a preparation method of a long-acting anti-sticking coating, which comprises the following steps:
(1) Adding deionized water, thickener hydroxyethyl cellulose and perfluoropolyether diol into a closed reaction kettle, slowly stirring by using an electric stirrer, slowly heating, and adding rutile type sodiumTiO rice 2 Repeatedly sanding, adding a defoaming agent, starting an electric stirrer to drive a stirring rod to rotate, uniformly stirring the liquid, adding a chlorine photosensitive polyamic acid emulsion, standing and cooling, continuously adding a polyisocyanate prefabricated object, and adjusting the pH value of the liquid to obtain a product A;
(2) Respectively adding fluorine-silicon modified polyester resin, a hydrophobic restoring agent and a mildew-proof algaecide, placing the mixture into a reaction kettle sealed in a dark environment for reaction for 2 hours, stirring and mixing the mixture, placing the mixture into a reaction kettle at 45-50 ℃ for heat preservation reaction for 30 minutes, after the mixture is cooled to 35 ℃ and the room temperature condition, dropwise adding secondary aminosilane into the reaction liquid, continuously introducing ammonia gas, and standing the mixture for 20 minutes after the dropwise adding is finished to obtain a product B;
(3) And (3) mixing the product A and the product B according to the weight ratio of 4 to 10:1, adding a cross-linking agent and an organic solvent into a reaction kettle, dispersing and fusing, and generating a-NCO-containing terminated fluorine-containing prepolymer by a-NCO group in a polyisocyanate preform and a-OH group in perfluoropolyether diol; reacting the-NCO-terminated fluorine-containing prepolymer with-NH-groups in secondary aminosilane to form-Si (OM) at two ends of a molecular chain 3 Hydrolysis to form-Si (OM) 3 End-capped polymers exposed to moisture in air, -Si (OH) after construction 3 The long-acting anti-sticking coating is obtained by dehydration condensation and curing to generate a three-dimensional cross-linked structure with higher hardness and better stability, and filtering and discharging after 10-20 min.
Further, the preparation method of the long-acting anti-sticking coating comprises the following components: 25-50 parts of deionized water, 0.2-0.3 part of thickener polyhydroxyethyl cellulose and 15-22 parts of rutile type nano TiO 2 1-3 parts of defoaming agent, 35-55 parts of chlorine photosensitive polyamic acid latex, 1.3-2.1 parts of flatting agent, 40-60 parts of perfluoropolyether diol and 40-60 parts of polyisocyanate preform; 3.5-5 parts of secondary aminosilane, 40-45 parts of fluorine-silicon modified polyester resin, 0.5-2 parts of hydrophobic restoring agent and 0.8-2.9 parts of mildew-proof and algae-proof agent.
Further, the preparation method of the long-acting anti-sticking coating comprises the following step of mixing one or more of isothiazolinone, benzimidazole, iodopropargyl, substituted aromatic hydrocarbon and dithiocarbamate; the defoaming agent is an organic silicon defoaming agent.
Furthermore, the fluorine-silicon modified polyester resin contains hydroxyl, the fluorine-silicon resin with hydroxyl and the branched chain type polyester resin with hydroxyl active groups are connected together through dehydration and polycondensation to form the fluorine-silicon modified polyester resin containing hydroxyl, and the hydroxyl value of the fluorine-silicon modified polyester resin is 50-150 mg of KOH.
Further, in the preparation method of the long-acting anti-sticking coating, the fluorine-silicon modified polyester resin comprises one or more of organosilicon modified hydroxyl acrylic resin, polysiloxane resin, hydroxyl acrylic resin, tetrafluoro resin and polyester resin.
Further, the preparation method of the long-acting anti-sticking coating comprises the following steps of preparing a polyisocyanate prefabricated object, wherein the polyisocyanate prefabricated object comprises one or more of HDI tripolymer, MDI tripolymer, IPDI tripolymer and TDI tripolymer; the thickener polyhydroxyethyl cellulose comprises one or more of methyl cellulose and ethyl cellulose; the perfluoropolyether diol comprises one or more compounds of K type perfluoropolyether, Y type perfluoropolyether, Z type perfluoropolyether and D type perfluoropolyether; the hydrophobic restoring agent is HSP-50 silane hydrophobic restoring agent.
Further, the preparation method of the long-acting anti-sticking coating comprises the following steps of mixing a product A and a product B according to a ratio of 4 to 10:1 into a reaction kettle, comprising: reacting fluorine-silicon modified polyester resin with polyisocyanate prepolymer for crosslinking and curing to generate a coating film with strong weather resistance, mixing a thickening agent of polyhydroxyethyl cellulose with rutile type nano TiO2, stirring the liquid uniformly, adding chlorine photosensitive polyamic acid emulsion, and adjusting the pH value of the liquid to generate the hydrophobic fluorocarbon coating.
Further, the preparation method of the long-acting anti-sticking coating comprises the step of preparing one of the crosslinking agents including one or more of isocyanurate, biuret, polyisocyanate, isocyanate trimer, biuret modification and isocyanate modification.
Further, the preparation method of the long-acting anti-sticking coatingMethod of the rutile type nano TiO 2 Ti-O octahedrons are arranged in a chain shape in a mode of sharing edges.
Further, the preparation method of the long-acting anti-sticking coating comprises the step of preparing the long-acting anti-sticking coating, wherein the flatting agent comprises one or more of polyacrylic acid and carboxymethyl cellulose.
The application provides a preparation method of a long-acting anti-sticking coating, which has the following beneficial effects:
(1) preparing-NCO end capping fluorine-containing prepolymer by polyisocyanate prefabricated object and perfluoropolyether diol, in a reaction kettle, completely consuming-NCO groups by chemical reaction of-NCO groups in-NCO end capping fluorine-containing prepolymer and-NH-groups of secondary aminosilane, and consuming-Si (OM) at two ends of molecular chain 3 Hydrolysis to form-Si (OH) 3 form-Si (OM) 3 End-capped polymers exposed to moisture in air after construction, -Si (OH) 3 The components (F, si) for reducing the surface energy in the molecular main chain are connected through chemical bonds, so that the problem that effective components are not gradually separated out along with the increase of the service time is solved, and the coating has excellent stability and durability;
(2) Adding rutile type nano TiO through thickener polyhydroxyethyl cellulose 2 After the liquid is uniformly stirred, the chlorine photosensitive polyamic acid emulsion is added, the PH value of the liquid is adjusted to generate the fluorocarbon coating, the hydrophobicity of the coating is increased, the problem that rainwater enters the interior of a wall along the coating in rainy and snowy weather is solved, the coating falls off due to the fact that the coating is adsorbed by rainwater to wash the coating after long-time use is solved, the adsorption force between the coating and the wall is enhanced, and the coating is effectively prevented from falling off from the wall under the action of external force to influence the use of the coating.
Drawings
FIG. 1 is a flow chart of a method of preparing a long-lasting release coating according to an embodiment of the present disclosure;
FIG. 2 is a graph showing the comparison of the experimental results of the long-lasting anti-adhesion coating of the examples and comparative examples in the present application;
the implementation, functional features and advantages of the present application will be further explained with reference to the accompanying drawings.
Detailed description of the preferred embodiments
In order to more clearly and completely describe the technical scheme of the invention, the invention is further described with reference to the accompanying drawings.
Referring to fig. 1-2, the present invention provides a preparation method of a long-acting anti-adhesion coating, comprising: the method comprises the following steps:
s1: adding deionized water, thickening agent polyhydroxyethyl cellulose and perfluoropolyether diol into a closed reaction kettle, stirring by using an electric stirrer, slowly heating to 65 ℃, and then adding rutile type nano TiO 2 Repeatedly sanding to 30mm, adding a defoaming agent, starting an electric stirrer to drive a stirring rod to rotate, uniformly stirring the liquid at the rotating speed of 1000 revolutions per minute, adding 37 parts of chlorine photosensitive polyamic acid emulsion, standing, cooling to 30 ℃, continuously adding the polyisocyanate preform, and adjusting the pH value of the liquid to 7.5 to obtain a product A;
s2: respectively adding fluorine-silicon modified polyester resin, a hydrophobic restoring agent and a mildew-proof algaecide, placing the mixture into a reaction kettle sealed in a dark environment for soaking reaction for 2 hours to ensure that the coating has a good surface protection effect on water-soluble dirt, oily dirt, charged dust, biological fungi and the like, stirring, mixing, placing the mixture at 45-50 ℃ for heat preservation reaction for 30 minutes, after cooling to 35 ℃ at room temperature, dropwise adding secondary amino silane into the reaction liquid, continuously introducing ammonia gas for reaction to prevent amino reduction, and standing for 20 minutes after dropwise adding is completed to obtain a product B;
s3: and (3) mixing the product A and the product B according to the weight ratio of 4 to 10:1, adding a cross-linking agent and an organic solvent into a reaction kettle, dispersing and fusing, and generating a-NCO-containing terminated fluorine-containing prepolymer by a-NCO group in a polyisocyanate preform and a-OH group in perfluoropolyether diol; reacting the-NCO-terminated fluorine-containing prepolymer with-NH-groups in secondary aminosilane to form-Si (OM) at two ends of a molecular chain 3 Hydrolysis to form-Si (OM) 3 End-capped polymers exposed to moisture in air after construction, -Si (OH) 3 Dewatering and condensing, curing to obtain three-dimensional cross-linked structure with high hardness and good stability, and filtering after 10-20minObtaining the long-acting anti-sticking coating;
the product A comprises the following components in parts by weight: 15-30 parts of deionized water, 0.2-0.3 part of thickener polyhydroxyethyl cellulose and 15-22 parts of rutile type nano TiO 2 1-3 parts of defoaming agent, 35-55 parts of chlorine photosensitive polyamic acid latex, 1.3-2.1 parts of flatting agent, 40-60 parts of perfluoropolyether diol and 40-60 parts of polyisocyanate preform;
the product B comprises the following components in parts by weight: 15-30 parts of deionized water, 3.5-5 parts of secondary aminosilane, 40-45 parts of fluorine-silicon modified polyester resin, 0.5-2 parts of hydrophobic restoring agent and 0.8-2.9 parts of mildew-proof and algae-proof agent.
In this example, a preparation method of a long-acting anti-sticking coating, a polyisocyanate preform and perfluoropolyether diol are prepared into-NCO terminated fluorine-containing prepolymer according to-NCO group and-OH group, F element is introduced into isocyanate molecule main chain, after product A and product B are placed into a reaction kettle, preparing the-NCO end capping fluorine-containing prepolymer and the secondary aminosilane according to-NCO group and-NH-group, completely consuming-NCO group through chemical reaction of-NCO end capping fluorine-containing prepolymer and-NH-group in the secondary aminosilane, and-Si (OM) at two ends of molecular chain 3 Hydrolysis to form-Si (OH) 3 form-Si (OM) 3 End-capped polymers exposed to moisture in air, -Si (OH) after construction 3 The components (F, si) for reducing the surface energy are connected through chemical bonds in the molecular main chain, so that the problem that effective components are not gradually separated out along with the increase of the service time is solved, and the coating has excellent stability and durability.
In this embodiment, a preparation method of a long-acting anti-sticking coating, fluorine-silicon modified polyester resin and polyisocyanate prepolymer are cross-linked and cured to form a coating film with strong hydrophobicity, oleophobicity, stain resistance, self-cleaning property and weather resistance, so that the problem that the coating is blown by wind and rain in outdoor environment is solved, and the application field is wide.
In this embodiment, a method for preparing a long-acting anti-adhesive coating, the anti-mold and anti-algae agent is one or a mixture of several of isothiazolinone, benzimidazole, iodopropargyl, substituted aromatic and dithiocarbamate; the flatting agent is an acrylate flatting agent; the defoaming agent is an organic silicon defoaming agent.
In this example, the fluorine-silicon modified polyester resin contains hydroxyl groups, and the hydroxyl group-containing fluorine-silicon modified polyester resin is formed by connecting a fluorine-silicon resin having hydroxyl groups and a branched polyester resin having hydroxyl active groups by dehydration polycondensation, and the hydroxyl value of the fluorine-silicon modified polyester resin is 50 to 150mg of KOH.
In the preparation method of the long-acting anti-adhesive coating in this embodiment, the fluorosilicone modified polyester resin is one or more of an organosilicon modified hydroxy acrylic resin, a polysiloxane resin, a hydroxy acrylic resin, a tetrafluoro resin, and a polyester resin.
In this embodiment, a method for preparing a long-acting anti-adhesion coating, the polyisocyanate preform is one of HDI trimer, MDI trimer, IPDI trimer and TDI trimer; the thickener polyhydroxyethyl cellulose can be methyl cellulose and ethyl cellulose; the perfluoropolyether diol comprises one or more compounds of K type perfluoropolyether, Y type perfluoropolyether, Z type perfluoropolyether and D type perfluoropolyether; the hydrophobic recovery agent is HSP-50 silane hydrophobic recovery agent; rutile type nano TiO 2 Ti-O octahedrons are arranged in a mode of sharing edges to form a chain shape, so that the refractive index is large, and the degradation of macromolecules is slowed down.
In the method for preparing the long-acting anti-adhesion coating in this embodiment, one of the crosslinking agents includes one or more of isocyanurate, biuret, polyisocyanate, isocyanate trimer, biuret modification, and isocyanate modification.
A construction method of a long-acting anti-sticking coating comprises the following steps:
s1, cleaning the surface of a base material, removing residual paint films, rust, oil stains, oxide scales and sundries on the surface of the base material, ensuring that the surface of the base material is free of rust, oil stains, dust and water marks, and then coating a layer of primer on the surface of the base material;
s2, after the surface of the primer is dried and cured, weighing the components according to the composition of the component A and the component B, respectively mixing the component A and the component B uniformly, and then mixing the component A and the component B according to the mass ratio of 4-10: 1 to obtain a finish, uniformly spraying the first surface paint on a primer until the first surface paint is dried and cured, wherein the dry film thickness of the primer is 50-60 um, the dry film thickness of the finish is 50-60 um, the construction temperature is 10-35 ℃, and the relative humidity of air is less than or equal to 75 percent.
Example 1:40 parts of deionized water, 0.2 part of thickener polyhydroxyethyl cellulose and 15 parts of rutile type nano TiO 2 1.2 parts of a defoaming agent, 37 parts of chlorine photosensitive polyamic acid latex, 1.3 parts of a flatting agent, 42 parts of perfluoropolyether diol and 45 parts of a polyisocyanate prefabricated product; 3.5 parts of secondary aminosilane, 40 parts of fluorine-silicon modified polyester resin, 1.2 parts of hydrophobic restoring agent and 0.5 part of mildew-proof and algae-proof agent;
s1: adding 20 parts of deionized water, 0.2 part of thickening agent polyhydroxyethyl cellulose and 42 parts of perfluoropolyether diol into a closed reaction kettle, stirring by using an electric stirrer, slowly heating the mixture to 65 ℃ in a hot water bath, and adding 15 parts of rutile type nano TiO 2 Repeatedly sanding to 30mm, adding 1.2 parts of defoaming agent, starting an electric stirrer to drive a stirring rod to rotate, uniformly stirring the liquid at the rotation speed of 1000 revolutions per minute, adding 37 parts of chlorine photosensitive polyamic acid emulsion, standing and cooling to 30 ℃, continuously adding 45 parts of polyisocyanate prefabricated product, and adjusting the pH value of the liquid to 7.5 to obtain a product A;
s2: respectively adding 20 parts of deionized water, 40 parts of fluorine-silicon modified polyester resin, 1.2 parts of hydrophobic restoring agent and 0.5 part of mildew-proof and algae-proof agent into a reaction kettle sealed in a dark environment, soaking and reacting for 2 hours to ensure that the coating has a good surface protection effect on water-soluble dirt, oily stain, charged dust, biological bacteria and the like, stirring, mixing, placing at 50 ℃ for heat preservation and reacting for 30 minutes, cooling to 35 ℃ at room temperature, dropwise adding 3.5 parts of secondary amine silane into the reaction liquid, continuously introducing ammonia gas for reacting to prevent amino reduction, and standing for 20 minutes to obtain a product B after dropwise adding is finished;
s3: the product A and the product B were prepared in the following manner of 6:1, adding a cross-linking agent and an organic solvent into a reaction kettle, and dispersing and fusingGenerating a fluorine-containing prepolymer containing a terminal-NCO end cap by an-NCO group in the cyanate preformed product and an-OH group in the perfluoropolyether diol; reacting-NCO end capping fluorine-containing prepolymer with-NH-group in secondary aminosilane to form-Si (OM) at two ends of molecular chain 3 Hydrolysis to form-Si (OM) 3 End-capped polymers exposed to moisture in air, -Si (OH) after construction 3 Dehydrating and condensing, curing to generate a three-dimensional cross-linked structure with higher hardness and better stability, and filtering and discharging after 10-20min to obtain the long-acting anti-sticking coating;
cleaning the surface of a base material, removing residual paint films, rust, oil stains, oxide scales and sundries on the surface of the base material, and coating a layer of primer on the surface of the base material after ensuring that the surface of the base material is free from rust, oil stains, dust and water marks;
after the surface of the primer is dried and cured, weighing the components according to the components A and B to obtain the finish paint, and uniformly spraying the finish paint on the primer with the thickness of 50 mu m until the primer is dried and cured.
Example 2:40 parts of deionized water, 0.3 part of thickener polyhydroxyethyl cellulose and 21 parts of rutile type nano TiO 2 1.2 parts of defoaming agent, 50 parts of chlorine photosensitive polyamic acid latex, 1.6 parts of flatting agent, 48 parts of perfluoropolyether diol and 55 parts of polyisocyanate preform; 4.2 parts of secondary aminosilane, 42 parts of fluorine-silicon modified polyester resin, 1.2 parts of hydrophobic restoring agent and 0.8 part of mildew-proof and algae-proof agent;
s1: adding 20 parts of deionized water, 0.3 part of thickening agent polyhydroxyethyl cellulose and 48 parts of perfluoropolyether diol into a closed reaction kettle, slowly stirring by using an electric stirrer, slowly heating to 65 ℃ in a hot water bath, and then adding 21 parts of rutile type nano TiO 2 Repeatedly sanding to 30mm, adding 1.2 parts of defoaming agent, starting an electric stirrer to drive a stirring rod to rotate, uniformly stirring the liquid at the rotating speed of 1000 revolutions per minute, adding 50 parts of chlorine photosensitive polyamic acid emulsion, standing, cooling to 30 ℃, continuously adding 55 parts of polyisocyanate prefabricated product, and adjusting the pH value of the liquid to 7.5 to obtain a product A;
s2: respectively adding 20 parts of deionized water, 42 parts of fluorine-silicon modified polyester resin, 1.2 parts of hydrophobic restoring agent and 0.8 part of mildew-proof and algae-proof agent, placing the mixture in a reaction kettle sealed in a dark environment for soaking reaction for 2 hours to ensure that the coating has a good surface protection effect on water-soluble dirt, oily stains, charged dust, biological bacteria and the like, stirring, mixing, placing the mixture at 45 ℃ for heat preservation reaction for 30 minutes, cooling the mixture to 35 ℃ at room temperature, dropwise adding 4.2 parts of secondary amine silane into the reaction solution, continuously introducing ammonia gas for reaction to prevent amino reduction, and standing the mixture for 20 minutes to obtain a product B after the dropwise adding is finished;
s3: the product A and the product B were prepared in the following manner of 6:1, adding a cross-linking agent and an organic solvent into a reaction kettle, dispersing and fusing, and generating a-NCO-containing terminated fluorine-containing prepolymer by a-NCO group in a polyisocyanate preform and a-OH group in perfluoropolyether diol; reacting-NCO end capping fluorine-containing prepolymer with-NH-group in secondary aminosilane to form-Si (OM) at two ends of molecular chain 3 Hydrolysis to form-Si (OM) 3 End-capped polymers exposed to moisture in air, -Si (OH) after construction 3 Dehydrating and condensing, curing to generate a three-dimensional cross-linked structure with higher hardness and better stability, and filtering and discharging after 10-20min to obtain the long-acting anti-sticking coating;
cleaning the surface of a base material, removing residual paint films, rust, oil stains, oxide scales and sundries on the surface of the base material, and coating a layer of primer on the surface of the base material after ensuring that the surface of the base material is free from rust, oil stains, dust and water marks;
after the surface of the primer is dried and cured, weighing the components according to the composition of the component A and the component B to obtain the finish paint, uniformly spraying the finish paint on the primer with the thickness of 50 mu m, and drying and curing.
Example 3:50 parts of deionized water, 0.28 part of thickener polyhydroxyethyl cellulose and 17 parts of rutile type nano TiO 2 1.2 parts of defoaming agent, 42 parts of chlorine photosensitive polyamic acid latex, 2.0 parts of flatting agent, 53 parts of perfluoropolyether diol and 49 parts of polyisocyanate preform; 3.8 parts of secondary aminosilane, 44 parts of fluorine-silicon modified polyester resin, 1.2 parts of hydrophobic restoring agent and 1.6 parts of mildew-proof and algae-proof agent;
s1: adding 25 parts of deionized water, 0.3 part of thickening agent polyhydroxyethyl cellulose and 53 parts of perfluoropolyether glycol into a closed reaction kettle to ensure thatSlowly stirring with electric stirrer, slowly heating to 65 deg.C in hot water bath, and adding 17 parts of rutile type nanometer TiO 2 Repeatedly sanding to 30mm, adding 1.2 parts of defoaming agent, starting an electric stirrer to drive a stirring rod to rotate, uniformly stirring the liquid at the rotating speed of 1000 revolutions per minute, adding 42 parts of chlorine photosensitive polyamic acid emulsion, standing, cooling to 30 ℃, continuously adding 49 parts of polyisocyanate prefabricated product, and adjusting the pH value of the liquid to 7.5 to obtain a product A;
s2: respectively adding 25 parts of deionized water, 44 parts of fluorine-silicon modified polyester resin, 1.2 parts of hydrophobic restoring agent and 1.6 parts of mildew-proof and algae-proof agent into a reaction kettle sealed in a dark environment for soaking reaction for 2 hours, so that the coating has a good surface protection effect on water-soluble dirt, oily dirt, charged dust, biological bacteria and the like, stirring, mixing, placing at 50 ℃ for heat preservation reaction for 30 minutes, cooling to 35 ℃ at room temperature, dropwise adding 3.8 parts of secondary amine silane into the reaction solution, continuously introducing ammonia gas for reaction to prevent amino reduction, and standing for 20 minutes after dropwise adding is completed to obtain a product B;
s3: the product A and the product B were prepared in the following manner: 1, putting the mixture into a reaction kettle, adding a cross-linking agent and an organic solvent, dispersing and fusing, and generating a-NCO-containing end-capped fluorine-containing prepolymer by a-NCO group in a polyisocyanate prefabricated product and a-OH group in perfluoropolyether diol; reacting the-NCO-terminated fluorine-containing prepolymer with-NH-groups in secondary aminosilane to form-Si (OM) at two ends of a molecular chain 3 Hydrolysis to form-Si (OM) 3 End-capped polymers exposed to moisture in air after construction, -Si (OH) 3 Dehydrating and condensing, curing to generate a three-dimensional cross-linked structure with higher hardness and better stability, and filtering and discharging after 10-20min to obtain the long-acting anti-sticking coating;
cleaning the surface of a base material, removing residual paint films, rust, oil stains, oxide scales and sundries on the surface of the base material, and coating a layer of primer on the surface of the base material after ensuring that the surface of the base material is free from rust, oil stains, dust and water marks;
after the surface of the primer is dried and cured, weighing the components according to the composition of the component A and the component B to obtain the finish paint, uniformly spraying the finish paint on the primer with the thickness of 50 mu m, and drying and curing.
Comparative example 1: the difference from example 1 is that the raw material of comparative example 1 does not contain rutile type nano TiO 2 。
Comparative example 2: the difference from example 1 is that the polyisocyanate preparation of comparative example 2 is replaced by an equal amount of dicyanate.
It can be seen from FIG. 2 that the raw material of comparative example 1 does not contain rutile type nano TiO 2 Containing rutile-type nano TiO 2 Compared with rutile-free nano TiO 2 The hydrophobicity of the examples 1 to 3 is also along with the rutile type nano TiO 2 The proportion of the component (A) is in direct proportion, and the component (B) contains rutile type nano TiO 2 The contact angle of the coating is increased, which shows that the hydrophobicity of the coating is enhanced, and the coating contains rutile type nano TiO 2 The fluorocarbon coating influences the strength and weakness of hydrophobicity.
Comparative example 2 the polyisocyanate preforms were replaced with equal amounts of dicyanate, the hardness, resistance to weathering and anti-graffiti effect of the polyisocyanate preforms used were poorer than those of the polyisocyanate preforms used, and the polyisocyanate preforms of examples 1-3 were proportional to the hardness, resistance to weathering and anti-graffiti effect.
It should be understood that the specific embodiments described herein are merely illustrative of and not restrictive on the broad application.
The technical solutions in the embodiments of the present application will be described clearly and completely with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all of the embodiments. All other embodiments obtained by a person of ordinary skill in the art based on the embodiments in the present application without making any creative effort belong to the protection scope of the present application.
In summary, a person skilled in the art can understand that all or part of the processes in the above-described method embodiments are implemented.
It should be noted that, in this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, apparatus, article, or method that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, apparatus, article, or method. Without further limitation, an element defined by the phrase "comprising one of 8230, and" comprising 8230does not exclude the presence of additional like elements in a process, apparatus, article, or method comprising the element.
The above description is only for the preferred embodiment of the present application and not intended to limit the scope of the present application, and all modifications of equivalent structures and equivalent processes, which are made by the contents of the specification and the drawings of the present application, or which are directly or indirectly applied to other related technical fields, are intended to be included within the scope of the present application.
Although embodiments of the present application have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the application, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. A preparation method of a long-acting anti-sticking coating is characterized by comprising the following steps:
(1) Adding deionized water, thickener hydroxyethyl cellulose and perfluoropolyether diol into a closed reaction kettle, slowly stirring by using an electric stirrer, slowly heating, and adding rutile type nano TiO 2 Repeatedly sanding, adding a defoaming agent, starting an electric stirrer to drive a stirring rod to rotate, uniformly stirring the liquid, adding a chlorine photosensitive polyamic acid emulsion, standing and cooling, continuously adding a polyisocyanate prefabricated object, and adjusting the pH value of the liquid to obtain a product A;
(2) Respectively adding fluorine-silicon modified polyester resin, a hydrophobic restoring agent and a mildew-proof algaecide, placing the mixture into a reaction kettle sealed in a dark environment for reaction for 2 hours, stirring and mixing the mixture, placing the mixture into a reaction kettle at 45-50 ℃ for heat preservation reaction for 30 minutes, after the mixture is cooled to 35 ℃ and the room temperature condition, dropwise adding secondary aminosilane into the reaction liquid, continuously introducing ammonia gas, and standing the mixture for 20 minutes after the dropwise adding is finished to obtain a product B;
(3) And (3) mixing the product A and the product B according to the weight ratio of 4-10: 1, adding a cross-linking agent and an organic solvent into a reaction kettle, dispersing and fusing, and generating a-NCO-containing terminated fluorine-containing prepolymer by a-NCO group in a polyisocyanate preform and a-OH group in perfluoropolyether diol; reacting the-NCO-terminated fluorine-containing prepolymer with-NH-groups in secondary aminosilane to form-Si (OM) at two ends of a molecular chain 3 Hydrolysis to form-Si (OM) 3 End-capped polymers exposed to moisture in air after construction, -Si (OH) 3 The long-acting anti-sticking coating is obtained by dehydration condensation and curing to generate a three-dimensional cross-linked structure with higher hardness and better stability, and filtering and discharging after 10-20 min.
2. The method for preparing a long-acting anti-sticking coating according to claim 1, comprising: 25-50 parts of deionized water, 0.2-0.3 part of thickener polyhydroxyethyl cellulose and 15-22 parts of rutile type nano TiO 2 1-3 parts of defoaming agent, 35-55 parts of chlorine photosensitive polyamic acid latex, 1.3-2.1 parts of flatting agent, 40-60 parts of perfluoropolyether diol, 40-60 parts of polyisocyanate preform, 3.5-5 parts of secondary aminosilane, 40-45 parts of fluorine-silicon modified polyester resin, 0.5-2 parts of hydrophobic restoring agent and 0.8-2.9 parts of mildew-proof and algae-proof agent.
3. The preparation method of the long-acting anti-sticking coating as claimed in claim 1, wherein the mildew-proof and anti-algae agent comprises one or a mixture of more of isothiazolinone, benzimidazole, iodopropargyl, substituted aromatic and dithiocarbamate; the defoaming agent is an organic silicon defoaming agent.
4. The preparation method of the long-acting anti-sticking coating according to claim 2, wherein the fluorine-silicon modified polyester resin contains hydroxyl groups, the fluorine-silicon resin with hydroxyl groups and the branched-chain polyester resin with hydroxyl active groups are connected together by dehydration polycondensation to form the fluorine-silicon modified polyester resin containing hydroxyl groups, and the hydroxyl value of the fluorine-silicon modified polyester resin is 50-150 mg KOH.
5. The method for preparing a long-acting anti-sticking coating according to claim 4, wherein the fluorosilicone modified polyester resin comprises one or more of silicone modified hydroxy acrylic resin, polysiloxane resin, hydroxy acrylic resin, tetrafluoro resin and a polyester resin.
6. The method of claim 2, wherein the polyisocyanate preform comprises one or more of HDI trimer, MDI trimer, IPDI trimer and TDI trimer; the thickener polyhydroxyethyl cellulose comprises one or more of methyl cellulose and ethyl cellulose; the perfluoropolyether diol comprises one or more compounds of K type perfluoropolyether, Y type perfluoropolyether, Z type perfluoropolyether and D type perfluoropolyether; the hydrophobic restoring agent is HSP-50 silane hydrophobic restoring agent.
7. The preparation method of the long-acting anti-sticking coating as claimed in claim 1, wherein the ratio of the product A to the product B is 4 to 10:1 into a reaction kettle, comprising: the fluorine-silicon modified polyester resin reacts with the polyisocyanate prepolymer for crosslinking and curing to generate a coating film with strong weather resistance, and the thickener of polyhydroxyethyl cellulose mixed with rutile type nano TiO 2 After the liquid is stirred uniformly, the chlorine photosensitive polyamic acid emulsion is added, and the PH value of the liquid is adjusted to obtain the hydrophobic fluorocarbon coating.
8. The method of claim 2, wherein the cross-linking agent comprises one or more of isocyanurate, biuret, polyisocyanate, isocyanate trimer, biuret modification, and isocyanate modification.
9. According to claim 1The preparation method of the long-acting anti-sticking coating is characterized in that the rutile type nano TiO 2 Ti-O octahedrons are arranged in a chain shape in a mode of sharing edges.
10. The method for preparing a long-acting anti-sticking coating according to claim 1, wherein the leveling agent comprises one or both of polyacrylic acid and carboxymethyl cellulose.
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