Preparation method of environment-friendly thermal insulation coating

Abstract

The application discloses a preparation method of an environment-friendly heat-insulating and heat-preserving coating, and the specific steps of the method are as follows: 1) preparing potassium hexatitanate whiskers through a droplet template technology: dissolving oxalic acid in deionized water to obtain A; adding titanium salt and potassium salt into A and stirring to obtain B; adding B into polyvinylpyrrolidone, ethylene glycol and tetrahydrofuran, stirring and aging to obtain a uniform film; heating under the condition of nitrogen to obtain single-crystal potassium hexatitanate; placing the single-crystal potassium hexatitanate in an alumina crucible, heating, quenching between two thick copper plates and cooling in liquid nitrogen; passing oxygen through the sample to obtain potassium hexatitanate whiskers through annealing; 2) preparing the environment-friendly heat-insulating and heat-preserving coating: mixing water, a dispersing agent, a wetting agent, ethylene glycol and a defoaming agent, adding hydroxyethyl cellulose and a pH regulator, further adding potassium hexatitanate whiskers and nano-silica aerogel and dispersing, and sequentially adding a water-based high-elastic emulsion, a water-based silicone-acrylate emulsion, a film-forming aid, a flame retardant, micrometer hollow glass microbeads, a bactericide and a near-infrared reflective material and stirring uniformly.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of heat preservation coating preparation, in particular to an environment-friendly heat preservation coating and a preparation method thereof. BACKGROUND

[0002] Energy competition is increasingly fierce, in order to effectively alleviate the energy problem, energy saving and consumption reduction become an important task of industrial enterprises, and it is essential to take heat preservation measures for equipment and pipelines.

[0003] Heat preservation coating combines the double characteristics of coating and heat preservation material, has many advantages, such as simple coating production process, low thermal conductivity, significant heat preservation effect, relatively simple construction, and is particularly suitable for replacing heat preservation materials to solve the heat preservation of special-shaped equipment. Heat preservation coating has the physical and chemical properties of coating and the characteristics of heat preservation material, which is a good complementary advantage to simultaneously exert the characteristics of both. Heat preservation coating is basically composed of four parts: base material, pigment and filler, solvent and additive. However, traditional coatings are mostly low solid content solvent type, containing a large amount of organic solvent, and many organic solvents need to be added for dilution during use. These solvents are volatilized into the atmosphere during construction and paint film drying, which is not only harmful to human health and pollutes the environment, but also flammable and has the risk of causing fire. According to the statistical data released by the National Bureau of Statistics, the total output of coatings in China reached 1648.188 million tons in 2014, an increase of 7.87% compared with the previous year. Compared with the total output of 1303.349 million tons in 2013, 344.839 million tons were added in 2014, setting a new historical high. With the increasingly strict environmental protection regulations in the world, the improvement of people's environmental protection consciousness, the perfection of environmental protection regulations and the popularization of environmental protection concept, the development of environment-friendly coatings is the trend. Environment-friendly heat preservation products with excellent heat preservation performance are increasingly recognized by consumers.

[0004] The development of environment-friendly nano heat preservation material technology with excellent heat preservation, environmental protection and energy saving, the combination of inorganic nano material and inorganic heat insulation material, and the preparation of a slurry heat insulation material with adjustable thermal performance by adding film forming and functional additives. This heat preservation and energy saving technology and material can greatly improve the heat insulation effect of inorganic materials, and has excellent environmental protection and fireproof performance. Potassium hexatitanate whisker has the advantages of stability, non-toxicity, high infrared reflectivity, low thermal conductivity and long service life, and can withstand high temperature of 800℃.

[0005] To this end, the present application provides a kind of preparation method of environment-friendly thermal insulation coating, first: by the liquid drop template of polymer stabilization is oriented to control single crystal potassium hexatitanate, polymer stabilization liquid drop template can not only adjust the single crystal structure of potassium hexatitanate, and also can be controlled by the definition of condition and morphology, the strategy not only provides the control volume change induced anisotropic directional morphology modulation intramuscular stress, but also makes ion not cross grain boundary.Compared with the potassium hexatitanate whisker synthesized by traditional method, the potassium hexatitanate whisker prepared by the method has a whisker structure, has a large specific surface area, so that it has a higher infrared reflectivity and a lower thermal conductivity, it has excellent high temperature resistance, thereby increasing the service life;At the same time, in the coating process, soft elastic anti-cracking technology is adopted, which effectively prevents the generation of wall cracks. SUMMARY

[0006] To achieve the above object, the present application provides the following technical scheme: a kind of preparation method of environment-friendly thermal insulation coating, comprising the following steps,

[0007] The preparation method of environment-friendly thermal insulation coating described in the present application. Its characterized in that the specific steps of the method are:

[0008] 1) liquid drop template technology preparation potassium hexatitanate whisker

[0009] (1) preparation of single crystal potassium hexatitanate: dissolve oxalic acid in deionized water, 60-80℃ under magnetic stirring for 1-2h, get solution A;Then organic titanium salt and soluble potassium salt are added to the above solution A, magnetic stirring for 1-2h, cool to room temperature to get solution B;B solution is added to the mixed solution of polyvinylpyrrolidone, ethylene glycol and tetrahydrofuran, wherein the volume ratio of the three is 12-10: 1: 1, then continue to stir for 2-3h, the obtained solution is cast on a 90mm culture dish, placed in an oven, aged at 100℃ for 48h, get polymer stabilized liquid drop template uniform film;The liquid drop template uniform film after orientation control is heated at 300-350℃ for 5-7h under inert gas nitrogen, and then heated at 650-750℃ for 8-10h, get single crystal potassium hexatitanate.

[0010] (2) preparation of potassium hexatitanate whisker: single crystal potassium hexatitanate is placed in high quality recrystallized alumina crucible, heated to 1100-1150℃ in resistance heating box furnace, kept for 20-24h, then plate quenching between two thick copper plates, then cooled with liquid nitrogen. Subsequently, the sample is annealed at 875-900℃ for 8-10 days under the condition of oxygen atmosphere (wherein the oxygen flow is 30-50sccm), get potassium hexatitanate whisker.

[0011] 2) preparation of environment-friendly thermal insulation coating

[0012] Mix 300 parts of water and 8 parts of dispersant, 3 parts of wetting agent non-ionic hydroxyl-containing copolymer, 8 parts of ethylene glycol, 2 parts of antifoaming agent evenly, add 2 parts of hydroxyethyl cellulose, 3 parts of pH regulator 2-amino-2-methyl-1-propanol, stir for 5-10 min to make it dissolve, then slowly add 80 parts of potassium titanate whisker and 30 parts of nano-silica aerogel (20-50 nm), and disperse at 1000-1500 r / min for 30-40 min, then reduce the speed, and then add 90 parts of water-based high-elastic emulsion acrylate emulsion, 100 parts of water-based silicone-acrylate emulsion, 8 parts of film-forming aid dodecanol ester, 200 parts of flame retardant, 100 parts of micron hollow glass beads (10-125 µm), 2 parts of bactericide biological enzyme and 2 parts of near-infrared reflective material, stir evenly, the total mixing time is 90-120 min, and the reaction temperature is 50-70 ℃.

[0013] Preferably, in the step (1), the organic titanium salt is one or a combination of tetrabutyl titanate, isopropyl titanate or tetraisopropyl titanate; and the soluble potassium salt is one or a combination of decarbonated potassium, potassium acetate or potassium oxalate.

[0014] Preferably, in the step (2), the oxygen flow rate of the oxygen atmosphere is 30-50 sccm.

[0015] Preferably, in the step (3), the dispersant is one or a combination of ammonium salt, sodium salt, phosphate salt and sulfonate salt; the flame retardant is one or a combination of low-density hexagonal flake-shaped magnesium hydroxide or aluminum hydroxide; and the near-infrared reflective material is one or a combination of indium tin oxide, antimony-doped tungsten acid zirconium, zinc sodium phosphate or bismuth molybdate.

[0016] Compared with the prior art, the environmentally friendly heat-insulating coating and the preparation method thereof have the following beneficial effects:

[0017] (1) The polymer-stable liquid droplet template is oriented to control the single crystal potassium titanate, the polymer-stable liquid droplet template technology can not only adjust the single crystal structure of the potassium titanate, but also control the pore structure and morphology through the definition of conditions, the strategy not only provides control of the anisotropic directional morphology modulation intramuscular stress induced by volume change, but also enables the ions not to cross the grain boundary, and further combines a simple growth technology and an internal stress growth mechanism to prepare potassium titanate nanowhiskers, so that the potassium titanate whiskers remain single crystals while having a whisker structure, and further have a small thermal conductivity; and the porous whisker structure makes it have better high-temperature resistance.

[0018] (2) Adopting soft elastic anti-cracking technology. The coating is added with water-based high-elastic emulsion, so that the coating has good elasticity, the elasticity modulus change index of each layer of wall body base layer is matched, the deformation and limitation deformation are combined, and the deformation stress can be dispersed and eliminated at any time. The base layer has strong deformation adaptability, and the generation of wall surface cracks is effectively prevented.

[0019] (3) Environment-friendly, the solvent used in the application is mainly water, and the pollution degree is greatly reduced. BRIEF DESCRIPTION OF DRAWINGS

[0020] Figure 1 SEM image of potassium titanate whisker in the embodiment of the application DETAILED DESCRIPTION

[0021] The technical solutions in the embodiments of the application will be clearly and completely described below with reference to the embodiments of the application. Obviously, the described embodiments are only part of the embodiments of the application, rather than all the embodiments of the application. Based on the embodiments in the application, all other embodiments obtained by those skilled in the art without creative labor fall within the protection scope of the application.

[0022] Embodiment one

[0023] 1) Preparation of potassium titanate whisker

[0024] (1) Preparation of single-crystal potassium titanate: oxalic acid is dissolved in deionized water, and the solution A is obtained by magnetic stirring at 60 ℃ for 2 h; then organic titanium tetrabutoxide and soluble potassium carbonate are added to the above solution A, and the solution B is obtained by magnetic stirring for 1 h and cooling to room temperature; the solution B is added to a mixed solution of polyvinylpyrrolidone, ethylene glycol and tetrahydrofuran, wherein the volume ratio of the three is 10:1:1, and then the stirring is continued for 2 h; the obtained solution is cast on a 90 mm culture dish and placed in an oven for aging at 100 ℃ for 48 h to obtain a uniform film; the uniform film is heated at 300 ℃ for 7 h and then heated at 650 ℃ for 10 h under the condition of inert gas nitrogen to obtain single-crystal potassium titanate.

[0025] (2) Potassium titanate whisker: the single-crystal potassium titanate is placed in a high-quality recrystallized alumina crucible, heated to 1100 ℃ in a resistance heating box furnace, kept for 24 h, and then plate quenching is performed between two thick copper plates, and then liquid nitrogen cooling is performed. Subsequently, the sample is annealed at 875 ℃ for 10 days under the condition of oxygen atmosphere (wherein the oxygen flow is 30 sccm) to obtain potassium titanate whisker.

[0026] 2) Preparation of environment-friendly heat-insulating and heat-preservation coating

[0027] Mix 300 parts of water and 8 parts of dispersant ammonium salt, 3 parts of wetting agent non-ionic hydroxyl-containing copolymer, 8 parts of ethylene glycol, 2 parts of defoaming agent uniformly, add 2 parts of hydroxyethyl cellulose, 3 parts of pH regulator 2-amino-2-methyl-1-propanol, stir for 5 min to dissolve, then slowly add 80 parts of potassium titanate whisker 30 parts of nano-silica aerogel (20 nm) after 1500 r / min dispersion for 30 min, reduce the speed, then add 90 parts of water-based high-elastic emulsion acrylate emulsion, 100 parts of water-based silicone-acrylate emulsion, 8 parts of film-forming aid dodecanol ester, 200 parts of flame retardant hexagonal magnesium hydroxide, 100 parts of micron hollow glass microspheres (10 μm), 2 parts of bactericide biological enzyme and 2 parts of near-infrared reflective material indium tin oxide, stir uniformly, the total mixing time is 90 min, and the reaction temperature is 50℃.

[0028] Example two

[0029] 1) Preparation of potassium titanate whisker

[0030] (1) Preparation of single crystal potassium titanate: oxalic acid was dissolved in deionized water, and stirred at 80℃ for 1h to obtain solution A; then organic titanium acid isopropyl ester and soluble potassium acetate were added to solution A, and stirred for 1h, and then cooled to room temperature to obtain solution B; B solution was added to a mixed solution of polyvinylpyrrolidone, ethylene glycol and tetrahydrofuran, and the volume ratio of the three was 12:1:1, then the stirring was continued for 2h, and the obtained solution was cast on a 90mm culture dish, and placed in an oven for aging at 100℃ for 48h to obtain a uniform film; the uniform film was heated at 350℃ for 5h and then at 750℃ for 8h under the condition of inert gas nitrogen to obtain single crystal potassium titanate.

[0031] (2) Potassium titanate whisker: single crystal potassium titanate was placed in a high-quality recrystallized alumina crucible, heated to 1150℃ in a resistance heating box furnace, kept for 20h, then plate quenching was carried out between two thick copper plates, and then cooled with liquid nitrogen. Subsequently, the sample was annealed at 900℃ for 8 days under the condition of oxygen atmosphere (wherein the oxygen flow was 50sccm) to obtain potassium titanate whisker.

[0032] 2) Preparation of environment-friendly thermal insulation coating

[0033] Mix 300 parts of water and 8 parts of dispersant sodium salt, 3 parts of wetting agent nonionic hydroxyl-containing copolymer, 8 parts of ethylene glycol, 2 parts of antifoaming agent, 2 parts of hydroxyethyl cellulose, 3 parts of pH regulator 2-amino-2-methyl-1-propanol, stir for 5 minutes to dissolve, then slowly add 80 parts of potassium titanate whisker, 30 parts of nano-silica aerogel (30 nm), and disperse at 1500 r / min for 30 minutes. After reducing the speed, add 90 parts of water-based high-elastic emulsion acrylate emulsion, 100 parts of water-based silicone-acrylate emulsion, 8 parts of film-forming aid dodecanol ester, 200 parts of flame retardant hexagonal magnesium hydroxide, 100 parts of micron hollow glass microbeads (50 μm), 2 parts of bactericide biological enzyme, and 2 parts of near-infrared reflective material antimony-doped zirconium tungstate, and stir uniformly. The total mixing time is 90 minutes, and the reaction temperature is 50°C.

[0034] Example Three

[0035] 1) Preparation of potassium titanate whisker

[0036] (1) Preparation of single-crystal potassium titanate: oxalic acid was dissolved in deionized water under magnetic stirring at 60°C for 2 hours to obtain solution A; then organic titanium acid ethyl ester and soluble potassium oxalate were added to solution A under magnetic stirring for 1 hour, and then cooled to room temperature to obtain solution B; solution B was added to a mixed solution of polyvinylpyrrolidone, ethylene glycol, and tetrahydrofuran in a volume ratio of 10:1:1, and then stirring was continued for 2 hours. The obtained solution was cast on a 90 mm petri dish and placed in an oven for aging at 100°C for 48 hours to obtain a uniform film; the uniform film was heated at 300°C for 7 hours and then at 650°C for 10 hours under the condition of inert gas nitrogen to obtain single-crystal potassium titanate.

[0037] (2) Potassium titanate whisker: single-crystal potassium titanate was placed in a high-quality recrystallized alumina crucible and heated to 1150°C in a resistance-heated box furnace for 20 hours, and then plate quenching was performed between two thick copper plates, and then liquid nitrogen cooling was performed. Subsequently, the sample was annealed at 875°C for 10 days under the condition of oxygen gas atmosphere (wherein the oxygen flow was 50 sccm) to obtain potassium titanate whisker.

[0038] 2) Preparation of environmentally friendly thermal insulation coating

[0039] Mix 300 parts of water and 8 parts of dispersant phosphate salt, 3 parts of wetting agent non-ionic hydroxyl-containing copolymer, 8 parts of ethylene glycol, 2 parts of defoaming agent evenly, add 2 parts of hydroxyethyl cellulose, 3 parts of pH regulator 2-amino-2-methyl-1-propanol stirring 5 min to make it dissolve, then slowly add 80 parts of potassium titanate whisker 30 parts of nano silica aerogel (50 nm) after 1500 r / min dispersion 30 min, reduce the speed, add 90 parts of water-based high-elastic emulsion acrylate emulsion, 100 parts of water-based silicone-acrylate emulsion, 8 parts of film-forming aid dodecanol ester, 200 parts of flame retardant aluminum hydroxide, 100 parts of micron hollow glass beads (70 μm), 2 parts of bactericide biological enzyme and 2 parts of near-infrared reflective material indium tin oxide, stirring evenly, the total mixing time is 100 min, the reaction temperature is 60℃.

[0040] Table 1 Performance index of environment-friendly thermal insulation coating

[0041]

Claims

1. A method for preparing an environmentally friendly thermal insulation coating, characterized in that, The specific steps of the method are: 1) Preparation of potassium hexatitanate whiskers by droplet template technology (1) Preparation of single crystal potassium hexatitanate: dissolve oxalic acid in deionized water, and magnetically stir at 60-80°C for 1-2h to obtain solution A; Then add organic titanium salt and soluble potassium salt to the above solution A, and magnetically stir for 1-2h, and cool to room temperature to obtain solution B; Add solution B to a mixed solution of polyvinylpyrrolidone, ethylene glycol and tetrahydrofuran, wherein the volume ratio of the three is 12-10:1:1, then continue to stir for 2-3h, and pour the obtained solution on a 90mm culture dish, and place it in an oven at 100°C for 48h to obtain a uniform polymer-stabilized droplet template film; Heat the polymer-stabilized droplet template uniform film under the condition of inert gas nitrogen at 300-350°C for 5-7h and then continue to heat at 650-750°C for 8-10h to obtain single crystal potassium hexatitanate; (2) Preparation of potassium hexatitanate whiskers: place the single crystal potassium hexatitanate in a recrystallized alumina crucible, heat to 1100-1150°C in a resistance-heated box furnace, and maintain for 20-24h, then perform plate splicing quenching between two copper plates, then cool with liquid nitrogen, and then anneal at 875-900°C for 8-10 days in an oxygen atmosphere to obtain potassium hexatitanate whiskers; 2) Preparation of environmentally friendly thermal insulation coating (3) Mix 300 parts of water with 8 parts of dispersant, 3 parts of wetting agent nonionic hydroxyl-containing copolymer, 8 parts of ethylene glycol, and 2 parts of defoaming agent uniformly, add 2 parts of hydroxyethyl cellulose and 3 parts of pH adjuster 2-amino-2-methyl-1-propanol and stir for 5-10min to dissolve them, then slowly add 80 parts of potassium hexatitanate whiskers and 30 parts of nano-silica aerogel and disperse for 30-40min at 1000-1500r / min, then reduce the speed, and add 90 parts of water-based high-elastic emulsion acrylate emulsion, 100 parts of water-based silicone-acrylate emulsion, 8 parts of film-forming aid dodecanol ester, 200 parts of flame retardant, 100 parts of micron hollow glass microbeads, 2 parts of bactericide biological lysozyme, and 2 parts of near-infrared reflective material in sequence, stir uniformly, the total mixing time is 90-120min, and the reaction temperature is 50-70°C, wherein the particle size of the nano-silica aerogel is 20-50nm, and the particle size of the micron hollow glass microbeads is 10-125μm.

2. The preparation method of the environment-friendly thermal insulation coating according to claim 1, characterized in that, In step (1), the organic titanium salt is one or a combination of tetrabutyl titanate, isopropyl titanate, or tetraisopropyl titanate; and the soluble potassium salt is one or a combination of potassium carbonate, potassium acetate, or potassium oxalate.

3. The preparation method of the environment-friendly thermal insulation coating according to claim 1, characterized in that, In step (2), the oxygen flow rate when the oxygen atmosphere is introduced is 30-50sccm.

4. The preparation method of the environment-friendly thermal insulation coating according to claim 1, characterized in that, In step (3), the dispersant is one or a combination of ammonium salt, sodium salt, phosphate ester salt, and sulfonate salt; the flame retardant is one or a combination of low-density hexagonal flaky magnesium hydroxide or aluminum hydroxide; and the near-infrared reflective material is one or a combination of indium tin oxide, antimony-doped zirconium tungstate, zinc sodium phosphate, or bismuth molybdate.

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