CN114163922A - Water-based nano heat-insulating coating and preparation method thereof - Google Patents
Water-based nano heat-insulating coating and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a water-based nano heat-insulating and heat-insulating coating and a preparation method thereof, wherein the coating prepared by the preparation method comprises components such as acrylic polyurethane emulsion, a dispersing agent, a defoaming agent, a wetting agent, a film-forming auxiliary agent, a pH regulator, a heat-insulating filler and the like, and has particularly excellent heat-insulating and heat-insulating properties; according to the scheme, fluorine and silicon monomers are introduced into the acrylate emulsion during preparation, so that the corrosion resistance of the coating can be improved, the hydrophobicity and the chemical medium resistance of the coating are excellent, the cross-linking sites among the coatings can be improved, the cross-linking density of each component is improved, the adhesive force between the coating and a base material can be improved, and the barrier property of a corrosive medium is further improved. The invention has reasonable process design and proper component proportion, and when the coating is coated on the surface of a pipeline, the coating has excellent heat preservation and insulation effects, hydrophobic surface, excellent corrosion resistance and higher practicability.
Description
Technical Field
The invention relates to the technical field of heat-insulating coatings, in particular to a water-based nano heat-insulating coating and a preparation method thereof.
Background
Energy competition is intensified day by day, the energy problem also becomes a bottleneck restricting economic development of China, and in order to effectively relieve the energy problem, energy conservation and consumption reduction become important tasks of industrial enterprises, heat preservation and insulation measures are necessary to be taken on equipment and pipelines. At present, most industrial temperature-carrying equipment adopts a wrapped heat insulation mode for heat insulation, the heat insulation system has the problems of high heat conductivity coefficient, easy moisture absorption of heat insulation materials, complex wrapping process, poor heat insulation effect and the like in the actual use process, and the research and development of heat insulation coatings are imperative.
The heat-insulating coating integrates the dual characteristics of the coating and the heat-insulating material, and has the advantages of simple production process, low heat conductivity coefficient, obvious heat-insulating effect, relatively simple construction, and the like, and is particularly suitable for heat insulation of special-shaped equipment which is difficult to replace the heat-insulating material. The heat-insulating coating has the physical and chemical properties of the coating and the characteristics of a heat-insulating material, and the excellent advantage complementation is beneficial to simultaneously playing the characteristics of the coating and the heat-insulating material. The heat-insulating paint is basically composed of four parts of base material (film-forming material), pigment and filler, solvent and adjuvant. The film-forming substances and pigments and fillers are decisive for the performance of the coating and are the basis of the coating system. As for the coating, the base material (film forming material) can be formed into a film alone or adhered with substances such as pigments and fillers, so that the quality of the base material directly influences the quality of the coating and the combination of the base material and the pigments and fillers.
At present, the variety of heat-insulating coatings on the market is various, but when the coatings disclosed at present are applied to the surface of an equipment pipeline, the heat-insulating effect is good, but the adhesive force between the coatings and the equipment pipeline cannot meet the requirements of people, and after the coatings work for a period of time in a high-temperature environment, the coatings are easy to separate from the surface of the pipeline, so that the heat-insulating effect is affected.
Disclosure of Invention
The invention aims to provide a water-based nano heat-insulating and heat-insulating coating and a preparation method thereof, so as to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme:
a preparation method of a water-based nano heat-insulating paint comprises the following steps:
(1) taking an emulsifier and deionized water, and uniformly mixing to obtain an emulsified aqueous solution;
uniformly mixing 1/2 parts of emulsified aqueous solution, 1/2 parts of ammonium persulfate and 2/3 parts of comonomer to obtain solution A; the comonomer comprises acrylate monomer, fluorine monomer and organosilicon monomer;
uniformly mixing 1/2 parts of emulsified aqueous solution, 1/2 parts of ammonium persulfate, 1/3 parts of comonomer, sodium bicarbonate and nitrogen, reacting at 75-80 ℃ for 3-4h, slowly dropwise adding the solution A for 1.5-2h, reacting at 75-80 ℃ for 4-6h under the condition of heat preservation, heating to 85-88 ℃, reacting at the temperature of 1-1.2h, cooling to 45 ℃, and adjusting the pH to 7 to obtain an acrylate emulsion;
(2) uniformly mixing diisocyanate, polyester diol, dimethylolpropionic acid and N, N-dimethylformamide, and heating to 65-70 ℃ for reacting for 8-10h to obtain a polyurethane prepolymer;
uniformly mixing the polyurethane prepolymer and the acrylate emulsion, and reacting at 70-75 ℃ for 6-8h to obtain acrylic polyurethane emulsion;
(3) taking acrylic polyurethane emulsion, adding a dispersing agent, a defoaming agent and a wetting agent under a shearing state, stirring for 20-30min, adding a film-forming assistant and a pH regulator, stirring for 20-30min, adding a heat-insulating filler, and stirring and dispersing for 30-50min at 500r/min under 300-.
According to an optimized scheme, in the step (1), the mass ratio of the acrylate monomer to the fluorine monomer to the organosilicon monomer is 15: 3: 2;
the acrylate monomer comprises butyl acrylate, methyl methacrylate, hydroxyethyl acrylate and acrylic acid, and the mass ratio of the butyl acrylate to the methyl methacrylate to the hydroxyethyl acrylate to the acrylic acid is 4: 3: 1: 2;
the organic silicon monomer comprises octamethylcyclotetrasiloxane, dimethyldiethoxysilane and 3-mercaptopropylmethyldiethoxysilane, wherein the mass ratio of the octamethylcyclotetrasiloxane to the dimethyldiethoxysilane to the 3-mercaptopropylmethyldiethoxysilane is 1: 1: 3.
according to an optimized scheme, the preparation method of the fluorine monomer comprises the following steps: taking sodium hydroxide and tetrahydrofuran, mixing uniformly, adding trifluoroethanol in nitrogen atmosphere, reacting for 1-1.2h at 28-30 ℃, cooling to 0 ℃, adding a mixed solution of pentafluorostyrene and tetrahydrofuran, continuing to react for 1-1.2h, heating to 70-75 ℃, performing reflux reaction for 16-18h, cooling after reaction, quenching with ice water, extracting an organic phase, washing with saturated saline water, and purifying to obtain the fluorine monomer.
According to an optimized scheme, the mol ratio of the pentafluorostyrene to the trifluoroethanol to the sodium hydroxide is 1: 1: 2.
according to an optimized scheme, in the step (1), the emulsifier comprises sodium dodecyl sulfate and OP-10, and the mass ratio of the emulsifier to the emulsifier is 1: 1; the dosage of the emulsifier is 3-4% of the total mass of the comonomer; the initiator accounts for 0.4-0.6% of the total mass of the comonomer; the dosage of the sodium bicarbonate is 10 percent of the mass of the emulsifier.
According to a more optimized scheme, in the step (2), the mass ratio of diisocyanate to polyester diol to dimethylolpropionic acid to N, N-dimethylformamide is 10: 5: 2: 30, of a nitrogen-containing gas; the mass ratio of the polyurethane prepolymer to the acrylate emulsion is 5: 3.
according to an optimized scheme, in the step (3), the components comprise, by mass, 75% of acrylic polyurethane emulsion, 0.5% of dispersing agent, 0.2% of defoaming agent, 0.2% of wetting agent, 0.5% of film-forming assistant, 0.1% of pH regulator and 23.5% of heat insulation filler.
According to an optimized scheme, the heat insulation filler comprises pretreated hollow glass beads, silica aerogel powder and graphene oxide, and the mass ratio of the pretreated hollow glass beads to the silica aerogel powder to the graphene oxide is 3: 1: 1.
according to an optimized scheme, the preparation steps of the pretreated hollow glass beads are as follows: putting hollow glass microspheres into 10% sodium hydroxide solution, soaking for 10-15h, taking out the hollow glass microspheres, mixing with ethanol and deionized water, ultrasonically dispersing for 20-30min, adding a silane coupling agent KH-590, stirring and reacting for 4-5h at 30-35 ℃, filtering, washing, and drying at 60-70 ℃ to obtain the pretreated hollow glass microspheres.
According to an optimized scheme, the coating is prepared by the preparation method of the water-based nano heat-insulating and heat-insulating coating.
Compared with the prior art, the invention has the following beneficial effects:
the invention discloses a water-based nano heat-insulating and heat-insulating coating and a preparation method thereof, wherein the coating prepared by the preparation method comprises components such as acrylic polyurethane emulsion, a dispersing agent, a defoaming agent, a wetting agent, a film-forming auxiliary agent, a pH regulator, a heat-insulating filler and the like, and has particularly excellent heat-insulating and heat-insulating properties; according to the scheme, the acrylic polyurethane emulsion is introduced, fluorine and silicon monomers are introduced into the acrylic emulsion during preparation, the introduction of the fluorine and silicon monomers can improve the corrosion resistance of the coating, the hydrophobicity and the chemical medium resistance of the coating are excellent, crosslinking sites among the coating can be improved, the crosslinking density of each component is improved, the adhesive force between the coating and a base material can be improved, and the barrier property of a corrosive medium is further improved.
On the basis of the scheme, because the coating prepared by the method is mainly used for coating the surface of the pipeline, the pipeline is mostly made of metal and alloy materials, after the actual coating is coated, the adhesion force of the pipeline and the coating is poor, the coating is easy to separate from the surface of the pipeline after being used at a high temperature for a period of time, and the heat insulation effect is greatly reduced, so that aiming at the problem, a mercapto monomer is introduced into the acrylic polyurethane emulsion by the method, and the coating is prepared by taking octamethylcyclotetrasiloxane, dimethyldiethoxysilane and 3-mercaptopropylmethyldiethoxysilane as organic silicon monomers in a mass ratio of 1: 1: 3', under the limitation of the parameter, the introduction of the sulfydryl can enable the adhesive force between the acrylic polyurethane emulsion and the surface of the pipeline to be greatly enhanced, and the use of the coating is ensured.
Meanwhile, the fluorine monomer is introduced, different from the conventional fluorine monomer, pentafluorostyrene is used as a raw material, sodium hydroxide is used as alkali, the sodium hydroxide and trifluoroethanol react to generate the fluorine monomer, the fluorine monomer introduces a benzene ring into a system, the thermal stability of the fluorine monomer is more excellent, the paint can still keep excellent adhesive force and heat insulation effect under a high-temperature environment, and the water resistance and corrosion resistance of the paint are excellent due to the introduction of fluorine.
The heat-insulating filler is prepared from pretreated hollow glass beads, silica aerogel powder and graphene oxide in a mass ratio of 3: 1: 1, the silicon dioxide aerogel is a super heat-insulating material which is researched more in recent years, and is a three-dimensional net-shaped porous structure formed by aggregating nano microspheres with the average particle size of 2-5nm, the size of a pore channel is 5-70nm, and the porosity can reach more than 90%; the hollow glass bead is a hollow, thin-wall and micron-sized inorganic nonmetal spherical powder material, and has the characteristics of small density, high strength, chemical inertness, good thermal stability, low heat conduction, low dielectric constant, sound insulation and the like; according to the application, the hollow glass beads, the silica aerogel powder and the graphene oxide are compounded through pretreatment, so that an excellent heat preservation and insulation effect is realized.
According to the scheme, the hollow glass microspheres are subjected to sulfhydrylation pretreatment, when in treatment, the hollow glass microspheres are soaked in 10% sodium hydroxide solution for 10-15 hours to improve the surface roughness, and then the surfaces of the hollow glass microspheres are subjected to sulfhydrylation treatment by using a silane coupling agent KH-590, so that on one hand, the sulfhydrylation treatment can improve the dispersibility of the hollow glass microspheres and avoid the agglomeration of the hollow glass microspheres so as to uniformly distribute heat insulation filler; on the other hand, due to the limitation of the metal material of the pipeline, the sulfhydrylation glass beads can be effectively attached to the surface of the pipeline to form a sulfhydrylation glass bead layer, and compared with the conventional three-material treatment, the heat insulation effect is more excellent.
The invention discloses a water-based nano heat-insulating coating and a preparation method thereof, the process design is reasonable, the component proportion is proper, the prepared coating has excellent adhesion performance, and when the coating is coated on the surface of a pipeline, the heat-insulating effect is excellent, the surface of the coating is hydrophobic, the corrosion resistance is excellent, and the practicability is higher.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic diagram of the actual coating effect of the coating prepared in example 1 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
a preparation method of a water-based nano heat-insulating paint comprises the following steps:
(1) taking sodium hydroxide and tetrahydrofuran, uniformly mixing, adding trifluoroethanol under the nitrogen atmosphere, reacting for 1.2h at 28 ℃, cooling to 0 ℃, adding a mixed solution of pentafluorostyrene and tetrahydrofuran, wherein the concentration of the mixed solution is 2mol/3L, continuing to react for 1h, heating to 70 ℃, carrying out reflux reaction for 18h, cooling after the reaction, quenching by ice water, extracting an organic phase, washing by saturated saline water, and purifying to obtain the fluorine monomer. The mol ratio of the pentafluorostyrene to the trifluoroethanol to the sodium hydroxide is 1: 1: 2.
taking an emulsifier and deionized water, and uniformly mixing to obtain an emulsified aqueous solution;
uniformly mixing 1/2 parts of emulsified aqueous solution, 1/2 parts of ammonium persulfate and 2/3 parts of comonomer to obtain solution A;
uniformly mixing 1/2 parts of emulsified aqueous solution, 1/2 parts of ammonium persulfate, 1/3 parts of comonomer, sodium bicarbonate and nitrogen, reacting for 4 hours at 75 ℃, slowly dropwise adding the solution A for 2 hours, keeping the temperature at 75 ℃ for reaction for 6 hours, heating to 85 ℃, keeping the temperature for reaction for 1.2 hours, cooling to 45 ℃, and adjusting the pH to 7 to obtain an acrylate emulsion;
wherein the comonomer comprises acrylate monomer, fluorine monomer and organosilicon monomer; the mass ratio of the acrylate monomer to the fluorine monomer to the organosilicon monomer is 15: 3: 2; the acrylate monomer comprises butyl acrylate, methyl methacrylate, hydroxyethyl acrylate and acrylic acid, and the mass ratio of the butyl acrylate to the methyl methacrylate to the hydroxyethyl acrylate to the acrylic acid is 4: 3: 1: 2; the organic silicon monomer comprises octamethylcyclotetrasiloxane, dimethyldiethoxysilane and 3-mercaptopropylmethyldiethoxysilane, wherein the mass ratio of the octamethylcyclotetrasiloxane to the dimethyldiethoxysilane to the 3-mercaptopropylmethyldiethoxysilane is 1: 1: 3.
the emulsifier comprises sodium dodecyl sulfate and OP-10, and the mass ratio of the sodium dodecyl sulfate to the OP-10 is 1: 1; the using amount of the emulsifier is 4% of the total mass of the comonomer; the initiator accounts for 0.6 percent of the total mass of the comonomer; the dosage of the sodium bicarbonate is 10 percent of the mass of the emulsifier.
(2) Uniformly mixing diisocyanate, polyester diol, dimethylolpropionic acid and N, N-dimethylformamide, and heating to 65 ℃ for reaction for 10 hours to obtain a polyurethane prepolymer; the mass ratio of diisocyanate to polyester diol to dimethylolpropionic acid to N, N-dimethylformamide is 10: 5: 2: 30, of a nitrogen-containing gas;
uniformly mixing the polyurethane prepolymer and the acrylate emulsion, and reacting at 70 ℃ for 8 hours to obtain acrylic polyurethane emulsion; the mass ratio of the polyurethane prepolymer to the acrylate emulsion is 5: 3.
(3) taking acrylic polyurethane emulsion, adding a dispersing agent, a defoaming agent and a wetting agent under a shearing state, stirring for 20min, adding a film-forming assistant and a pH regulator, stirring for 20min, adding a heat insulation filler, and stirring and dispersing for 30min at 500r/min to obtain a finished coating.
The heat-insulating coating comprises, by mass, 75% of acrylic polyurethane emulsion, 0.5% of a dispersing agent, 0.2% of a defoaming agent, 0.2% of a wetting agent, 0.5% of a film-forming aid, 0.1% of a pH regulator and 23.5% of a heat-insulating filler. The heat insulation filler comprises pretreated hollow glass beads, silica aerogel powder and graphene oxide, and the mass ratio of the pretreated hollow glass beads to the silica aerogel powder is 3: 1: 1.
the preparation method of the pretreated hollow glass bead comprises the following steps: putting hollow glass microspheres into a 10% sodium hydroxide solution, soaking for 10h, taking out the hollow glass microspheres, mixing with ethanol and deionized water, ultrasonically dispersing for 25min, adding a silane coupling agent KH-590, stirring and reacting for 4h at 35 ℃, filtering and washing, and drying at 65 ℃ to obtain the pretreated hollow glass microspheres. The silane coupling agent accounts for 5 wt% of the total weight of the hollow glass microspheres.
Example 2:
a preparation method of a water-based nano heat-insulating paint comprises the following steps:
(1) taking sodium hydroxide and tetrahydrofuran, uniformly mixing, adding trifluoroethanol under the nitrogen atmosphere, reacting for 1.1h at 29 ℃, cooling to 0 ℃, adding a mixed solution of pentafluorostyrene and tetrahydrofuran, wherein the concentration of the mixed solution is 2mol/3L, continuing to react for 1.1h, heating to 72 ℃, performing reflux reaction for 17h, cooling after reaction, quenching with ice water, extracting an organic phase, washing with saturated saline water, and purifying to obtain a fluorine monomer. The mol ratio of the pentafluorostyrene to the trifluoroethanol to the sodium hydroxide is 1: 1: 2.
taking an emulsifier and deionized water, and uniformly mixing to obtain an emulsified aqueous solution;
uniformly mixing 1/2 parts of emulsified aqueous solution, 1/2 parts of ammonium persulfate and 2/3 parts of comonomer to obtain solution A;
uniformly mixing 1/2 parts of emulsified aqueous solution, 1/2 parts of ammonium persulfate, 1/3 parts of comonomer, sodium bicarbonate and nitrogen, reacting for 3.5 hours at 78 ℃, slowly dropwise adding the solution A for 2 hours, keeping the temperature at 78 ℃ for 5 hours, heating to 87 ℃, keeping the temperature for reacting for 1.1 hour, cooling to 45 ℃, and adjusting the pH to 7 to obtain acrylic ester emulsion;
wherein the comonomer comprises acrylate monomer, fluorine monomer and organosilicon monomer; the mass ratio of the acrylate monomer to the fluorine monomer to the organosilicon monomer is 15: 3: 2; the acrylate monomer comprises butyl acrylate, methyl methacrylate, hydroxyethyl acrylate and acrylic acid, and the mass ratio of the butyl acrylate to the methyl methacrylate to the hydroxyethyl acrylate to the acrylic acid is 4: 3: 1: 2; the organic silicon monomer comprises octamethylcyclotetrasiloxane, dimethyldiethoxysilane and 3-mercaptopropylmethyldiethoxysilane, wherein the mass ratio of the octamethylcyclotetrasiloxane to the dimethyldiethoxysilane to the 3-mercaptopropylmethyldiethoxysilane is 1: 1: 3.
the emulsifier comprises sodium dodecyl sulfate and OP-10, and the mass ratio of the sodium dodecyl sulfate to the OP-10 is 1: 1; the using amount of the emulsifier is 4% of the total mass of the comonomer; the initiator accounts for 0.6 percent of the total mass of the comonomer; the dosage of the sodium bicarbonate is 10 percent of the mass of the emulsifier.
(2) Uniformly mixing diisocyanate, polyester diol, dimethylolpropionic acid and N, N-dimethylformamide, and heating to 68 ℃ for reaction for 9 hours to obtain a polyurethane prepolymer; the mass ratio of diisocyanate to polyester diol to dimethylolpropionic acid to N, N-dimethylformamide is 10: 5: 2: 30, of a nitrogen-containing gas;
uniformly mixing the polyurethane prepolymer and the acrylate emulsion, and reacting at 72 ℃ for 7 hours to obtain acrylic polyurethane emulsion; the mass ratio of the polyurethane prepolymer to the acrylate emulsion is 5: 3.
(3) taking acrylic polyurethane emulsion, adding a dispersing agent, a defoaming agent and a wetting agent under a shearing state, stirring for 25min, adding a film-forming assistant and a pH regulator, stirring for 25min, adding a heat insulation filler, and stirring and dispersing for 40min at 400r/min to obtain a finished coating.
The heat-insulating coating comprises, by mass, 75% of acrylic polyurethane emulsion, 0.5% of a dispersing agent, 0.2% of a defoaming agent, 0.2% of a wetting agent, 0.5% of a film-forming aid, 0.1% of a pH regulator and 23.5% of a heat-insulating filler. The heat insulation filler comprises pretreated hollow glass beads, silica aerogel powder and graphene oxide, and the mass ratio of the pretreated hollow glass beads to the silica aerogel powder is 3: 1: 1.
the preparation method of the pretreated hollow glass bead comprises the following steps: putting hollow glass microspheres into a 10% sodium hydroxide solution, soaking for 12h, taking out the hollow glass microspheres, mixing with ethanol and deionized water, ultrasonically dispersing for 25min, adding a silane coupling agent KH-590, stirring and reacting for 4h at 35 ℃, filtering and washing, and drying at 65 ℃ to obtain the pretreated hollow glass microspheres. The silane coupling agent accounts for 5 wt% of the total weight of the hollow glass microspheres.
Example 3:
a preparation method of a water-based nano heat-insulating paint comprises the following steps:
(1) taking sodium hydroxide and tetrahydrofuran, uniformly mixing, adding trifluoroethanol under the nitrogen atmosphere, reacting for 1h at 30 ℃, cooling to 0 ℃, adding a mixed solution of pentafluorostyrene and tetrahydrofuran, wherein the concentration of the mixed solution is 2mol/3L, continuing to react for 1.2h, heating to 75 ℃, refluxing for 16h, cooling after reaction, quenching with ice water, extracting an organic phase, washing with saturated saline water, and purifying to obtain the fluorine monomer. The mol ratio of the pentafluorostyrene to the trifluoroethanol to the sodium hydroxide is 1: 1: 2.
taking an emulsifier and deionized water, and uniformly mixing to obtain an emulsified aqueous solution;
uniformly mixing 1/2 parts of emulsified aqueous solution, 1/2 parts of ammonium persulfate and 2/3 parts of comonomer to obtain solution A;
uniformly mixing 1/2 parts of emulsified aqueous solution, 1/2 parts of ammonium persulfate, 1/3 parts of comonomer, sodium bicarbonate and nitrogen, reacting for 3 hours at 80 ℃, slowly dropwise adding the solution A for 2 hours, reacting for 4 hours at 80 ℃ under heat preservation, heating to 88 ℃, reacting for 1 hour under heat preservation, cooling to 45 ℃, and adjusting the pH to 7 to obtain an acrylate emulsion;
wherein the comonomer comprises acrylate monomer, fluorine monomer and organosilicon monomer; the mass ratio of the acrylate monomer to the fluorine monomer to the organosilicon monomer is 15: 3: 2; the acrylate monomer comprises butyl acrylate, methyl methacrylate, hydroxyethyl acrylate and acrylic acid, and the mass ratio of the butyl acrylate to the methyl methacrylate to the hydroxyethyl acrylate to the acrylic acid is 4: 3: 1: 2; the organic silicon monomer comprises octamethylcyclotetrasiloxane, dimethyldiethoxysilane and 3-mercaptopropylmethyldiethoxysilane, wherein the mass ratio of the octamethylcyclotetrasiloxane to the dimethyldiethoxysilane to the 3-mercaptopropylmethyldiethoxysilane is 1: 1: 3.
the emulsifier comprises sodium dodecyl sulfate and OP-10, and the mass ratio of the sodium dodecyl sulfate to the OP-10 is 1: 1; the using amount of the emulsifier is 4% of the total mass of the comonomer; the initiator accounts for 0.6 percent of the total mass of the comonomer; the dosage of the sodium bicarbonate is 10 percent of the mass of the emulsifier.
(2) Uniformly mixing diisocyanate, polyester diol, dimethylolpropionic acid and N, N-dimethylformamide, and heating to 70 ℃ for reacting for 8 hours to obtain a polyurethane prepolymer; the mass ratio of diisocyanate to polyester diol to dimethylolpropionic acid to N, N-dimethylformamide is 10: 5: 2: 30, of a nitrogen-containing gas;
uniformly mixing the polyurethane prepolymer and the acrylate emulsion, and reacting at 75 ℃ for 6 hours to obtain acrylic polyurethane emulsion; the mass ratio of the polyurethane prepolymer to the acrylate emulsion is 5: 3.
(3) taking acrylic polyurethane emulsion, adding a dispersing agent, a defoaming agent and a wetting agent under a shearing state, stirring for 30min, adding a film-forming assistant and a pH regulator, stirring for 30min, adding a heat insulation filler, and stirring and dispersing for 30min at 500r/min to obtain a finished coating.
The heat-insulating coating comprises, by mass, 75% of acrylic polyurethane emulsion, 0.5% of a dispersing agent, 0.2% of a defoaming agent, 0.2% of a wetting agent, 0.5% of a film-forming aid, 0.1% of a pH regulator and 23.5% of a heat-insulating filler. The heat insulation filler comprises pretreated hollow glass beads, silica aerogel powder and graphene oxide, and the mass ratio of the pretreated hollow glass beads to the silica aerogel powder is 3: 1: 1.
the preparation method of the pretreated hollow glass bead comprises the following steps: putting hollow glass microspheres into a 10% sodium hydroxide solution, soaking for 15h, taking out the hollow glass microspheres, mixing with ethanol and deionized water, ultrasonically dispersing for 25min, adding a silane coupling agent KH-590, stirring and reacting for 4h at 35 ℃, filtering, washing, and drying at 65 ℃ to obtain the pretreated hollow glass microspheres. The silane coupling agent accounts for 5 wt% of the total weight of the hollow glass microspheres.
In the above examples, the dispersant is a polycarboxylate dispersant, the defoamer is an organosilicon defoamer, the wetting agent is alkyl polyoxyethylene ether, and the coalescent is a dodecyl ester coalescent.
The control experiment was carried out using example 2 as the experimental group, as the following comparative example:
comparative example 1:
a preparation method of a water-based nano heat-insulating paint comprises the following steps:
(1) taking an emulsifier and deionized water, and uniformly mixing to obtain an emulsified aqueous solution;
uniformly mixing 1/2 parts of emulsified aqueous solution, 1/2 parts of ammonium persulfate and 2/3 parts of comonomer to obtain solution A;
uniformly mixing 1/2 parts of emulsified aqueous solution, 1/2 parts of ammonium persulfate, 1/3 parts of comonomer, sodium bicarbonate and nitrogen, reacting for 3.5 hours at 78 ℃, slowly dropwise adding the solution A for 2 hours, keeping the temperature at 78 ℃ for 5 hours, heating to 87 ℃, keeping the temperature for reacting for 1.1 hour, cooling to 45 ℃, and adjusting the pH to 7 to obtain acrylic ester emulsion;
wherein the comonomer comprises acrylate monomer and organosilicon monomer; the mass ratio of the acrylate monomer to the organosilicon monomer is 15: 2; the acrylate monomer comprises butyl acrylate, methyl methacrylate, hydroxyethyl acrylate and acrylic acid, and the mass ratio of the butyl acrylate to the methyl methacrylate to the hydroxyethyl acrylate to the acrylic acid is 4: 3: 1: 2; the organic silicon monomer comprises octamethylcyclotetrasiloxane, dimethyldiethoxysilane and 3-mercaptopropylmethyldiethoxysilane, wherein the mass ratio of the octamethylcyclotetrasiloxane to the dimethyldiethoxysilane to the 3-mercaptopropylmethyldiethoxysilane is 1: 1: 3.
the emulsifier comprises sodium dodecyl sulfate and OP-10, and the mass ratio of the sodium dodecyl sulfate to the OP-10 is 1: 1; the using amount of the emulsifier is 4% of the total mass of the comonomer; the initiator accounts for 0.6 percent of the total mass of the comonomer; the dosage of the sodium bicarbonate is 10 percent of the mass of the emulsifier.
In comparative example 1, no fluoromonomer was introduced, and the remaining process steps and parameters were in accordance with example 2.
Comparative example 2:
a preparation method of a water-based nano heat-insulating paint comprises the following steps:
(1) taking sodium hydroxide and tetrahydrofuran, uniformly mixing, adding trifluoroethanol under the nitrogen atmosphere, reacting for 1.1h at 29 ℃, cooling to 0 ℃, adding a mixed solution of pentafluorostyrene and tetrahydrofuran, wherein the concentration of the mixed solution is 2mol/3L, continuing to react for 1.1h, heating to 72 ℃, performing reflux reaction for 17h, cooling after reaction, quenching with ice water, extracting an organic phase, washing with saturated saline water, and purifying to obtain a fluorine monomer. The mol ratio of the pentafluorostyrene to the trifluoroethanol to the sodium hydroxide is 1: 1: 2.
taking an emulsifier and deionized water, and uniformly mixing to obtain an emulsified aqueous solution;
uniformly mixing 1/2 parts of emulsified aqueous solution, 1/2 parts of ammonium persulfate and 2/3 parts of comonomer to obtain solution A;
uniformly mixing 1/2 parts of emulsified aqueous solution, 1/2 parts of ammonium persulfate, 1/3 parts of comonomer, sodium bicarbonate and nitrogen, reacting for 3.5 hours at 78 ℃, slowly dropwise adding the solution A for 2 hours, keeping the temperature at 78 ℃ for 5 hours, heating to 87 ℃, keeping the temperature for reacting for 1.1 hour, cooling to 45 ℃, and adjusting the pH to 7 to obtain acrylic ester emulsion;
wherein the comonomer comprises acrylate monomer, fluorine monomer and organosilicon monomer; the mass ratio of the acrylate monomer to the fluorine monomer to the organosilicon monomer is 15: 3: 2; the acrylate monomer comprises butyl acrylate, methyl methacrylate, hydroxyethyl acrylate and acrylic acid, and the mass ratio of the butyl acrylate to the methyl methacrylate to the hydroxyethyl acrylate to the acrylic acid is 4: 3: 1: 2; the organosilicon monomer comprises octamethylcyclotetrasiloxane and dimethyldiethoxysilane, and the mass ratio of the octamethylcyclotetrasiloxane to the dimethyldiethoxysilane is 1: 1.
the emulsifier comprises sodium dodecyl sulfate and OP-10, and the mass ratio of the sodium dodecyl sulfate to the OP-10 is 1: 1; the using amount of the emulsifier is 4% of the total mass of the comonomer; the initiator accounts for 0.6 percent of the total mass of the comonomer; the dosage of the sodium bicarbonate is 10 percent of the mass of the emulsifier.
Comparative example 2 did not incorporate a mercapto monomer and the remaining process steps and parameters were consistent with example 2.
Comparative example 3:
a preparation method of a water-based nano heat-insulating paint comprises the following steps:
(3) taking acrylic polyurethane emulsion, adding a dispersing agent, a defoaming agent and a wetting agent under a shearing state, stirring for 25min, adding a film-forming assistant and a pH regulator, stirring for 25min, adding a heat insulation filler, and stirring and dispersing for 40min at 400r/min to obtain a finished coating.
The heat-insulating coating comprises, by mass, 75% of acrylic polyurethane emulsion, 0.5% of a dispersing agent, 0.2% of a defoaming agent, 0.2% of a wetting agent, 0.5% of a film-forming aid, 0.1% of a pH regulator and 23.5% of a heat-insulating filler. The heat insulation filler comprises hollow glass beads, silica aerogel powder and graphene oxide, and the mass ratio of the hollow glass beads to the silica aerogel powder is 3: 1: 1.
in comparative example 3, the glass beads were not pretreated, and the remaining process steps and parameters were the same as those in example 2.
Detection experiment:
the coatings prepared in examples 1-3 and comparative examples 1-3 were used for the following tests:
1. the adhesion A of the coating was tested according to GBT5210-2006 adhesion test Standard by paint and varnish Pull-off, where the test substrate was a steel plate and the coating thickness was 5 mm.
2. A test sample is prepared according to the scheme of the experiment 1, and is placed in 5% sodium hydroxide, 3% sodium chloride, 5% concentrated sulfuric acid and deionized water at room temperature, soaked for 240 hours, and the change condition of the surface coating is observed.
3. Test samples were prepared according to the protocol of experiment 1, one side of the sample was coated with a film and the film covered only 1/2 substrate, after the film was dried, the uncoated side of the sample was placed on a hot plate and heated to 120, 140, 150 ℃ until the uncoated side of the sample was at the temperature, and the surface temperature of the coating was recorded.
4. After testing according to the method of experiment 3, the paint is kept at 150 ℃ for 4h, cooled and retested for adhesion B.
And (4) conclusion: the invention discloses a water-based nano heat-insulating coating and a preparation method thereof, the process design is reasonable, the component proportion is proper, the prepared coating has excellent adhesion performance, and when the coating is coated on the surface of a pipeline, the heat-insulating effect is excellent, the surface of the coating is hydrophobic, the corrosion resistance is excellent, and the practicability is higher.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of a water-based nano heat-insulating paint is characterized by comprising the following steps: the method comprises the following steps:
(1) taking an emulsifier and deionized water, and uniformly mixing to obtain an emulsified aqueous solution;
uniformly mixing 1/2 parts of emulsified aqueous solution, 1/2 parts of ammonium persulfate and 2/3 parts of comonomer to obtain solution A; the comonomer comprises acrylate monomer, fluorine monomer and organosilicon monomer;
uniformly mixing 1/2 parts of emulsified aqueous solution, 1/2 parts of ammonium persulfate, 1/3 parts of comonomer, sodium bicarbonate and nitrogen, reacting at 75-80 ℃ for 3-4h, slowly dropwise adding the solution A, reacting at 75-80 ℃ for 4-6h under heat preservation, heating to 85-88 ℃, reacting at 1-1.2h under heat preservation, cooling to 45 ℃, and adjusting the pH value to 7 to obtain an acrylate emulsion;
(2) uniformly mixing diisocyanate, polyester diol, dimethylolpropionic acid and N, N-dimethylformamide, and heating to 65-70 ℃ for reacting for 8-10h to obtain a polyurethane prepolymer;
uniformly mixing the polyurethane prepolymer and the acrylate emulsion, and reacting at 70-75 ℃ for 6-8h to obtain acrylic polyurethane emulsion;
(3) taking acrylic polyurethane emulsion, adding a dispersing agent, a defoaming agent and a wetting agent under a shearing state, stirring for 20-30min, adding a film-forming assistant and a pH regulator, stirring for 20-30min, adding a heat-insulating filler, and stirring and dispersing for 30-50min at 500r/min under 300-.
2. The preparation method of the water-based nano heat-insulating and heat-insulating coating as claimed in claim 1, wherein the preparation method comprises the following steps: in the step (1), the mass ratio of the acrylate monomer to the fluorine monomer to the organosilicon monomer is 15: 3: 2;
the acrylate monomer comprises butyl acrylate, methyl methacrylate, hydroxyethyl acrylate and acrylic acid, and the mass ratio of the butyl acrylate to the methyl methacrylate to the hydroxyethyl acrylate to the acrylic acid is 4: 3: 1: 2;
the organic silicon monomer comprises octamethylcyclotetrasiloxane, dimethyldiethoxysilane and 3-mercaptopropylmethyldiethoxysilane, wherein the mass ratio of the octamethylcyclotetrasiloxane to the dimethyldiethoxysilane to the 3-mercaptopropylmethyldiethoxysilane is 1: 1: 3.
3. the preparation method of the water-based nano heat-insulating and heat-insulating coating as claimed in claim 2, characterized in that: the preparation method of the fluorine monomer comprises the following steps: taking sodium hydroxide and tetrahydrofuran, mixing uniformly, adding trifluoroethanol in nitrogen atmosphere, reacting for 1-1.2h at 28-30 ℃, cooling to 0 ℃, adding a mixed solution of pentafluorostyrene and tetrahydrofuran, continuing to react for 1-1.2h, heating to 70-75 ℃, performing reflux reaction for 16-18h, cooling after reaction, quenching with ice water, extracting an organic phase, washing with saturated saline water, and purifying to obtain the fluorine monomer.
4. The preparation method of the water-based nano heat-insulating and heat-insulating coating as claimed in claim 3, wherein the preparation method comprises the following steps: the mol ratio of the pentafluorostyrene to the trifluoroethanol to the sodium hydroxide is 1: 1: 2.
5. the preparation method of the water-based nano heat-insulating and heat-insulating coating as claimed in claim 1, wherein the preparation method comprises the following steps: in the step (1), the emulsifier comprises sodium dodecyl sulfate and OP-10, and the mass ratio of the sodium dodecyl sulfate to the OP-10 is 1: 1; the dosage of the emulsifier is 3-4% of the total mass of the comonomer; the initiator accounts for 0.4-0.6% of the total mass of the comonomer; the dosage of the sodium bicarbonate is 10 percent of the mass of the emulsifier.
6. The preparation method of the water-based nano heat-insulating and heat-insulating coating as claimed in claim 1, wherein the preparation method comprises the following steps: in the step (2), the mass ratio of diisocyanate, polyester diol, dimethylolpropionic acid and N, N-dimethylformamide is 10: 5: 2: 30, of a nitrogen-containing gas; the mass ratio of the polyurethane prepolymer to the acrylate emulsion is 5: 3.
7. the preparation method of the water-based nano heat-insulating and heat-insulating coating as claimed in claim 1, wherein the preparation method comprises the following steps: in the step (3), the components comprise, by mass, 75% of acrylic polyurethane emulsion, 0.5% of dispersing agent, 0.2% of defoaming agent, 0.2% of wetting agent, 0.5% of film-forming assistant, 0.1% of pH regulator and 23.5% of heat-insulating filler.
8. The preparation method of the water-based nano heat-insulating and heat-insulating coating as claimed in claim 1, wherein the preparation method comprises the following steps: the heat insulation filler comprises pretreated hollow glass beads, silica aerogel powder and graphene oxide, wherein the mass ratio of the pretreated hollow glass beads to the silica aerogel powder to the graphene oxide is 3: 1: 1.
9. the preparation method of the water-based nano heat-insulating and heat-insulating coating as claimed in claim 8, wherein the preparation method comprises the following steps: the preparation method of the pretreated hollow glass bead comprises the following steps: putting hollow glass microspheres into 10% sodium hydroxide solution, soaking for 10-15h, taking out the hollow glass microspheres, mixing with ethanol and deionized water, ultrasonically dispersing for 20-30min, adding a silane coupling agent KH-590, stirring and reacting for 4-5h at 30-35 ℃, filtering, washing, and drying at 60-70 ℃ to obtain the pretreated hollow glass microspheres.
10. The coating prepared by the preparation method of the water-based nano heat-insulating and heat-insulating coating according to any one of claims 1 to 9.
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