CN115073981B - Preparation method of water-based nano heat-preservation heat-insulation coating - Google Patents

Preparation method of water-based nano heat-preservation heat-insulation coating Download PDF

Info

Publication number
CN115073981B
CN115073981B CN202210607606.6A CN202210607606A CN115073981B CN 115073981 B CN115073981 B CN 115073981B CN 202210607606 A CN202210607606 A CN 202210607606A CN 115073981 B CN115073981 B CN 115073981B
Authority
CN
China
Prior art keywords
heat
titanium dioxide
nano
parts
water
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202210607606.6A
Other languages
Chinese (zh)
Other versions
CN115073981A (en
Inventor
谢松洋
李先民
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Beijing Longyuan Naxin Technology Co ltd
Original Assignee
Beijing Longyuan Naxin Technology Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Beijing Longyuan Naxin Technology Co ltd filed Critical Beijing Longyuan Naxin Technology Co ltd
Priority to CN202210607606.6A priority Critical patent/CN115073981B/en
Publication of CN115073981A publication Critical patent/CN115073981A/en
Application granted granted Critical
Publication of CN115073981B publication Critical patent/CN115073981B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D133/00Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/004Reflecting paints; Signal paints
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/18Fireproof paints including high temperature resistant paints
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/61Additives non-macromolecular inorganic
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/32Phosphorus-containing compounds
    • C08K2003/321Phosphates
    • C08K2003/328Phosphates of heavy metals

Landscapes

  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Paints Or Removers (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention relates to a preparation method of a water-based nanometer heat preservation and heat insulation coating, which comprises the following specific steps: 1) Dissolving titanium salt in a mixed solvent and uniformly stirring; reacting, cooling, washing and drying to disperse titanium dioxide nanoclusters; dispersing the titanium dioxide nano-sheet in a buffer solution, adding dopamine hydrochloride, stirring, filtering and calcining to obtain the controllable high-dispersion two-dimensional ultrathin titanium dioxide nano-sheet. 2) Preparing PVDF/(potassium carbonate and titanium dioxide) nanofiber felt; the potassium hexatitanate crystal/PVDF nanofiber felt is obtained through low-temperature treatment; pure O 2 is used as atmosphere, heating, sealing, cooling after keeping for 20-30 min, and collecting whisker samples. 3) Weighing raw materials, and preparing aqueous nano SiO 2 aerogel suspension emulsion; dispersing mica powder, adding near infrared reflecting material and fire retardant, and stirring; preparing synthetic slurry; adding aerogel suspension emulsion, synthetic slurry, film forming auxiliary agent and other auxiliary agents into a mixed product of materials such as mica powder, stirring at a low speed, obtaining the water-based nano heat-insulating coating, and coating and drying to obtain the coating.

Description

Preparation method of water-based nano heat-preservation heat-insulation coating
Technical Field
The invention relates to the technical field of heat preservation coating preparation, in particular to a novel water-based nanometer heat preservation heat-insulation coating and a preparation method thereof.
Background
The coating is a continuous film which is coated on the surface of the protected or decorated object and can form firm adhesion with the coated object, and is usually a viscous liquid prepared by using resin, oil or emulsion as main materials, adding or not adding pigment and filler, adding corresponding auxiliary agents and using organic solvent or water.
At present, along with the continuous improvement of the energy-saving requirements of buildings, the comfort requirements of people on living, working, learning, entertainment and other places are also continuously improved, and on the premise that the places are ensured to be warm in winter and cool in summer, the expenditure of energy use is also continuously reduced, and the heat-insulating coating is often required to be used for reforming the heat-insulating areas such as the existing building outer walls or roofs and the like, so that the outer walls have the functions of heat preservation, heat insulation and the like. However, the traditional building heat insulation material is mostly an organic heat insulation material, and has poor fireproof performance. In recent years, serious fire accidents of external heat preservation engineering of buildings continuously occur in China, the loss is serious, and serious influence is caused in the national range. Aiming at the major fire accidents, the living building department and the public security department clearly stipulate that the heat insulation and preservation material of the outer wall of the civil building in China must adopt a building with the combustion performance of A level or B1 level and the height of less than 24m, the combustion performance of the heat preservation material is not lower than B2 level, and meanwhile, the fireproof isolation belt is arranged, so that the application range of the traditional heat insulation and preservation material of the building in the building engineering is greatly limited. Inorganic heat-insulating materials, such as rock wool, mineral wool, glass wool, foam concrete, vitrified microbeads and the like, have poor heat conductivity and heat-insulating performance even fail when meeting water, and are difficult to achieve ideal heat-insulating and heat-insulating energy-saving effects when used alone, although the combustion performance reaches the A level.
The environment-friendly water-based nanometer heat-insulating material technology with excellent heat insulation, fireproof safety and environmental protection is developed, and the inorganic nanometer material and the inorganic heat-insulating material are compounded and matched with film forming and functional auxiliary agents to prepare the serous heat-insulating material with adjustable thermal performance. The heat insulation and energy conservation technology and the material can greatly improve the heat insulation and heat conservation effect of the inorganic material, and have excellent environmental protection and fireproof performance.
Therefore, the controllable high-dispersion two-dimensional ultrathin titanium dioxide nanosheets are added into the novel water-based nano heat-insulating coating, have larger specific surface area and more reaction sites, and can better improve the ageing resistance, heat insulation performance of the coating; in addition, the potassium hexatitanate whisker prepared by the nanofiber template-induced low-temperature heat treatment combined with the flowing oxygen-assisted thermal evaporation method has high yield, and has excellent high-temperature resistance compared with the potassium hexatitanate whisker synthesized by the traditional method. Therefore, the water-based nanometer heat-insulating coating prepared based on the two improved materials has the advantages of excellent heat insulation and heat preservation, fire prevention safety and environmental protection, and the service life of the coating is prolonged.
Disclosure of Invention
In order to achieve the above purpose, the present invention provides the following technical solutions: a novel water-based nanometer heat preservation and heat insulation coating and a preparation method thereof comprise the following steps,
The invention relates to a preparation method of a water-based nanometer heat preservation and heat insulation coating. The method is characterized by comprising the following specific steps:
1) Preparation of controllable high-dispersion two-dimensional double-layer ultrathin titanium dioxide nanosheets
(1) Dissolving titanium salt in a mixed solvent of ethylene glycol and deionized water, magnetically stirring for 10-20 min until the solution is uniformly mixed, transferring into a reaction kettle, reacting for 20-24 h at 200-240 ℃, cooling to room temperature, washing 3-5 times with deionized water and an organic solvent, and then placing in a vacuum drying oven for overnight drying at 100-120 ℃ to obtain dispersed titanium dioxide nanoclusters;
(2) Dispersing the titanium dioxide nanoclusters obtained in the step (1) in 100-150 mL of buffer solution, and then adding dopamine hydrochloride into the buffer solution, wherein the mass ratio of the titanium dioxide nanoclusters to the dopamine hydrochloride is (2-5): and 1, magnetically stirring the suspension for 24-30 h at room temperature, filtering, and calcining in a muffle furnace at a speed of 1-2 ℃/min at 400-500 ℃ for 3-5 h to finally obtain the controllable high-dispersion two-dimensional double-layer ultrathin titanium dioxide nanosheets.
2) Preparation of potassium hexatitanate whisker by nano-fiber template induced low-temperature heat treatment combined with flowing oxygen auxiliary thermal evaporation method
(1) Dissolving polyvinylidene fluoride in a mixed solvent of N, N-dimethylformamide and acetone, wherein the volume ratio of the N, N-dimethylformamide to the acetone is 1-3: 1, a step of; heating the solution to 50-55 ℃ until the polyvinylidene fluoride is completely dissolved;
(2) Adding potassium carbonate and titanium dioxide into the solution, continuously stirring to form a uniform solution, and preparing PVDF/(potassium carbonate and titanium dioxide) nanofiber felt by adopting an electrostatic spinning method under the voltage of 10-15 KV; the distance between the receiving plate and the spinning end is 10-15 cm;
(3) Carrying out low-temperature treatment on PVDF/(potassium carbonate and titanium dioxide) nanofiber felt at 140-180 ℃ for 12-24 hours to obtain potassium hexatitanate crystal powder/PVDF nanofiber felt;
(4) In order to improve the formation of potassium hexatitanate whisker, pure O 2 is adopted as flowing atmosphere, the flow speed is 6-8L/min, a pipe of aluminum oxide is heated to 600-750 ℃ in a muffle furnace, then potassium hexatitanate crystal powder/PVDF nanofiber felt is placed in the pipe of aluminum oxide to be sealed, the oxygen partial pressure is 50-60 KPa, the pipe is cooled to room temperature after being kept for 20-30 min, and a potassium hexatitanate whisker sample is collected through a membrane filter placed between a vacuum pipe and a vacuum pump.
3) Preparation of water-based nano heat-preservation heat-insulation coating
(1) Weighing the following raw materials in weight: 20 parts of solvent, 22 parts of acrylic weather-resistant emulsion, 10 parts of near infrared reflecting material, 10 parts of nano hollow glass beads, 10 parts of composite nano ceramic beads, 3.5 parts of SiO 2 aerogel, 3 parts of mica powder, 6 parts of potassium hexatitanate whisker, 10 parts of controllable high-dispersion two-dimensional ultrathin titanium dioxide nanosheets, 1 part of film forming auxiliary agent, 0.5 part of ultraviolet absorber, 2 parts of flame retardant and 2 parts of other auxiliary agents;
(2) Placing the acrylic emulsion and the SiO 2 aerogel into a sealed homogenizing emulsifying machine for stirring and mixing, so that the SiO 2 aerogel is fully dispersed, mixed and uniformly compounded in the emulsion to obtain a water-based nano SiO 2 aerogel suspension emulsion;
(3) Dispersing mica powder in a high-speed stirrer, and then placing the near infrared reflecting material and the flame retardant into the high-speed stirrer for continuous stirring until the materials are uniformly mixed;
(4) Loading the controllable high-dispersion two-dimensional ultrathin titanium dioxide nanosheets, potassium hexatitanate whiskers and a solvent into a sealed homogenizing emulsifying machine for high-speed shearing and grinding to obtain premixed slurry, adding nano hollow glass beads and composite nano ceramic beads into the prepared premixed slurry, and continuously stirring and mixing to fully disperse the controllable high-dispersion two-dimensional ultrathin titanium dioxide nanosheets, the nano hollow glass beads and the composite nano ceramic beads in the solvent, and uniformly mixing to obtain synthetic slurry;
(5) Adding the aqueous nano SiO 2 aerogel suspension emulsion, the synthetic slurry, the film forming auxiliary agent and other auxiliary agents into the product obtained in the step (3), stirring at a low speed, dispersing uniformly to obtain the aqueous nano heat-preserving heat-insulating coating, and coating and drying to obtain the nano heat-preserving heat-insulating coating.
Preferably, in the step 1), the titanium salt is one of tetrabutyl titanate, isopropyl titanate, or tetraisopropyl titanate, or a combination thereof.
Preferably, in the step 1), the volume ratio of the mixed solvent glycol to the deionized water is 2-3: 1.
Preferably, in the step 3), the solvent is a combination of deionized water, ethanol or n-butanol, wherein the weight ratio is as follows: 10: 5-8: 2 to 5.
Preferably, in the step 3), the acrylic acid is one or a combination of methacrylic acid and methyl methacrylate.
Preferably, in the step 3), the flame retardant is one or a combination of magnesium hydroxide or aluminum hydroxide with low density.
Preferably, in the step 3), the auxiliary agent is one or a combination of an antifoaming agent, a leveling agent and a stabilizer.
Preferably, in the step 3), the near infrared reflecting material is one or a combination of indium tin oxide, sodium zinc phosphate and bismuth molybdate.
Compared with the prior art, the preparation method for preparing the anti-dazzle nano antimicrobial composite functional material and the coating has the following beneficial effects:
(1) The titanium dioxide nanoclusters are prepared by a hydrothermal method, and the high dispersibility enables the titanium dioxide nanosheets to have high dispersity, so that the titanium dioxide heat preservation and insulation effects can be improved; the two-dimensional double-layer ultrathin titanium dioxide nanosheets have larger specific surface area and more reaction sites.
(2) The titanium atoms in the two-dimensional double-layer ultrathin titanium dioxide nanosheets are easy to form a certain complex with water molecules in the air due to the electronic arrangement, and hydrogen atoms in the ligand water molecules are easy to attract oxygen, nitrogen and the like in the air through Van der Waals force, so that the material has better slow conductivity on heat by air or inert gas in more closed spaces, the material changes very slowly along with external temperature change, and finally the heat preservation effect is achieved; meanwhile, the heat-insulating material has the effect of reflecting various rays and the like generating heat, and achieves the effect that the temperature of an acting surface does not rise rapidly along with the radiation of a heat source, thereby achieving the heat-insulating effect.
(3) The potassium hexatitanate whisker is prepared by combining low-temperature heat treatment induced by a nanofiber template with a flowing oxygen auxiliary thermal evaporation method, and potassium hexatitanate nanocrystal is prepared by low-temperature heat treatment induced by the nanofiber template, and potassium carbonate and titanium dioxide have higher reactivity mainly under the induction of the nanofiber template, so that the treatment temperature is reduced; and then the potassium hexatitanate whisker is prepared by a flowing oxygen auxiliary thermal evaporation method, the potassium hexatitanate nanocrystals are converted into potassium hexatitanate whisker, the yield of the potassium hexatitanate whisker prepared under severe conditions is high, and compared with the potassium hexatitanate whisker synthesized by the traditional method, the potassium hexatitanate whisker has excellent high temperature resistance, so that the service life is prolonged.
Drawings
FIG. 1 is an SEM image of a titanium dioxide nanocluster according to an embodiment of the present invention
FIG. 2 is an SEM image of potassium dititanate whiskers according to an embodiment of the invention
FIG. 3 is a process flow diagram of a water-based nano heat-insulating coating according to a first, second and third embodiment of the invention
FIG. 4 is a graph showing the effect of the thickness of the first, second and third intermediate coatings on the heat insulating properties of the material according to the embodiment of the present invention
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
1) Preparation of controllable high-dispersion two-dimensional double-layer ultrathin titanium dioxide nanosheets
(1) Tetrabutyl titanate is dissolved in a mixed solvent of glycol and deionized water, and the volume ratio of the glycol to deionized water is 3:1, magnetically stirring for 15min until the solution is uniformly mixed, transferring to a reaction kettle, reacting for 20h at 220 ℃, cooling to room temperature, washing 3 times with deionized water and an organic solvent, and then placing in a vacuum drying oven for overnight drying at 120 ℃ to obtain dispersed titanium dioxide nanoclusters;
(2) Dispersing the titanium dioxide nanoclusters obtained in the step (1) in 100mL of buffer solution, and then adding dopamine hydrochloride into the buffer solution, wherein the mass ratio of the titanium dioxide nanoclusters to the dopamine hydrochloride is 4: and 1, magnetically stirring the suspension for 24 hours at room temperature, filtering, and calcining in a muffle furnace at the speed of 2 ℃/min for 4 hours at the temperature of 450 ℃ to finally obtain the controllable high-dispersion two-dimensional double-layer ultrathin titanium dioxide nanosheets.
2) Preparation of potassium hexatitanate whisker by nano-fiber template induced low-temperature heat treatment combined with flowing oxygen auxiliary thermal evaporation method
(1) Dissolving polyvinylidene fluoride in a mixed solvent of N, N-dimethylformamide and acetone, wherein the volume ratio of the N, N-dimethylformamide to the acetone is 1:1, a step of; heating the solution to 50 ℃ until the polyvinylidene fluoride is completely dissolved;
(2) Adding potassium carbonate and titanium dioxide into the solution, continuously stirring to form a uniform solution, and preparing PVDF/(potassium carbonate and titanium dioxide) nanofiber felt by adopting an electrostatic spinning method under the voltage of 10 KV; and the distance between the receiving plate and the spinning end is 10cm;
(3) Carrying out low-temperature treatment on PVDF/(potassium carbonate and titanium dioxide) nanofiber felt at 140 ℃ for 20 hours to obtain potassium hexatitanate crystal powder/PVDF nanofiber felt;
(4) In order to improve the formation of potassium hexatitanate whisker, pure O 2 is adopted as flowing atmosphere, the flow speed is 6L/min, a tube of aluminum oxide is heated to 600 ℃ in a muffle furnace, then the potassium hexatitanate crystal powder/PVDF nanofiber felt is placed in the tube of aluminum oxide to be sealed, the oxygen partial pressure is 50KPa, the tube is cooled to room temperature after being kept for 20min, and a potassium hexatitanate whisker sample is collected through a membrane filter placed between a vacuum tube and a vacuum pump.
3) Preparation of water-based nano heat-preservation heat-insulation coating
(1) Weighing the following raw materials in weight: 20 parts of solvent (the solvent is a combination of deionized water, ethanol or n-butanol, wherein the weight ratio is 10:8:5), 22 parts of methacrylic acid weather-resistant emulsion, 10 parts of near infrared reflecting material indium tin oxide, 10 parts of nano hollow glass beads, 10 parts of composite nano ceramic beads, 3.5 parts of SiO 2 aerogel, 3 parts of mica powder, 6 parts of potassium hexatitanate whisker, 10 parts of controllable high-dispersion two-dimensional ultrathin titanium dioxide nanosheets, 1 part of film forming auxiliary agent, 0.5 part of ultraviolet absorbent, 2 parts of flame retardant low-density magnesium hydroxide and 2 parts of defoaming agent;
(2) Placing methacrylic acid emulsion and SiO 2 aerogel into a sealed homogenizing emulsifying machine for stirring and mixing, so that the SiO 2 aerogel is fully dispersed, mixed and uniformly compounded in the emulsion to obtain aqueous nano SiO 2 aerogel suspension emulsion;
(3) Dispersing mica powder in a high-speed stirrer, and then placing the near infrared reflecting material indium tin oxide and low-density magnesium hydroxide into the high-speed stirrer for continuous stirring until the materials are uniformly mixed;
(4) Loading the controllable high-dispersion two-dimensional ultrathin titanium dioxide nanosheets, potassium hexatitanate whiskers and a solvent into a sealed homogenizing emulsifying machine for high-speed shearing and grinding to obtain premixed slurry, adding nano hollow glass beads and composite nano ceramic beads into the prepared premixed slurry, and continuously stirring and mixing to enable the controllable high-dispersion two-dimensional ultrathin titanium dioxide nanosheets, the nano hollow glass beads and the composite nano ceramic beads to be fully dispersed and uniformly mixed in the solvent, so as to obtain synthetic slurry;
(5) Adding the aqueous nano SiO 2 aerogel suspension emulsion, the synthetic slurry, the film forming auxiliary agent and the defoaming agent into the product obtained in the step (3), stirring at a low speed, dispersing uniformly to obtain the aqueous nano heat-preserving heat-insulating coating, and coating and drying to obtain the nano heat-preserving heat-insulating coating with the thickness of 1mm.
Example two
1) Preparation of controllable high-dispersion two-dimensional double-layer ultrathin titanium dioxide nanosheets
(1) Dissolving isopropyl titanate in a mixed solvent of glycol and deionized water, wherein the volume ratio of the glycol to deionized water is 2:1, magnetically stirring for 10min until the solution is uniformly mixed, transferring to a reaction kettle, reacting at 200 ℃ for 24h, cooling to room temperature, washing with deionized water and an organic solvent for 3 times, and then placing in a vacuum drying oven for drying at 100 ℃ overnight to obtain dispersed titanium dioxide nanoclusters;
(2) Dispersing the titanium dioxide nanoclusters obtained in the step (1) in 100mL of buffer solution, and then adding dopamine hydrochloride into the buffer solution, wherein the mass ratio of the titanium dioxide nanoclusters to the dopamine hydrochloride is 2: and 1, magnetically stirring the suspension for 24 hours at room temperature, filtering, calcining in a muffle furnace at 400 ℃ for 5 hours at a speed of 1 ℃/min, and finally obtaining the controllable high-dispersion two-dimensional double-layer ultrathin titanium dioxide nanosheets.
2) Preparation of potassium hexatitanate whisker by nano-fiber template induced low-temperature heat treatment combined with flowing oxygen auxiliary thermal evaporation method
(1) Dissolving polyvinylidene fluoride in a mixed solvent of N, N-dimethylformamide and acetone, wherein the volume ratio of the N, N-dimethylformamide to the acetone is 2:1, a step of; heating the solution to 55 ℃ until the polyvinylidene fluoride is completely dissolved;
(2) Adding potassium carbonate and titanium dioxide into the solution, continuously stirring to form a uniform solution, and preparing PVDF/(potassium carbonate and titanium dioxide) nanofiber felt by adopting an electrostatic spinning method under the voltage of 15 KV; the distance between the receiving plate and the spinning end is 15cm;
(3) Carrying out low-temperature treatment on PVDF/(potassium carbonate and titanium dioxide) nanofiber felt at 160 ℃ for 18h to obtain potassium hexatitanate crystal powder/PVDF nanofiber felt;
(4) In order to improve the formation of potassium hexatitanate whisker, pure O 2 is adopted as flowing atmosphere, the flow speed is 8L/min, a tube of aluminum oxide is heated to 650 ℃ in a muffle furnace, then the potassium hexatitanate crystal powder/PVDF nanofiber felt is placed in the tube of aluminum oxide to be sealed, the oxygen partial pressure is 55KPa, the tube is cooled to room temperature after being kept for 20min, and a potassium hexatitanate whisker sample is collected through a membrane filter placed between a vacuum tube and a vacuum pump.
3) Preparation of water-based nano heat-preservation heat-insulation coating
(1) Weighing the following raw materials in weight: 20 parts of solvent (the solvent is the combination of deionized water, ethanol or n-butanol, wherein the weight ratio is 10:8:3), 22 parts of methyl methacrylate weather-resistant emulsion, 10 parts of near infrared reflecting material zinc sodium phosphate, 10 parts of nanoscale hollow glass beads, 10 parts of composite nano ceramic beads, 3.5 parts of SiO 2 aerogel, 3 parts of mica powder, 6 parts of potassium hexatitanate whisker, 10 parts of controllable high-dispersion two-dimensional ultrathin titanium dioxide nano sheet, 1 part of film forming auxiliary agent, 0.5 part of ultraviolet absorbent, 2 parts of flame retardant low-density aluminum hydroxide and 2 parts of advection agent;
(2) Placing the methyl methacrylate emulsion and the SiO 2 aerogel into a sealed homogenizing emulsifying machine for stirring and mixing, so that the SiO 2 aerogel is fully dispersed, mixed and uniformly compounded in the emulsion to obtain a water-based nano SiO 2 aerogel suspension emulsion;
(3) Dispersing mica powder in a high-speed stirrer, and then placing near infrared reflecting material zinc sodium phosphate and fire retardant low-density aluminum hydroxide into the high-speed stirrer for continuous stirring until the materials are uniformly mixed;
(4) Loading the controllable high-dispersion two-dimensional ultrathin titanium dioxide nanosheets, potassium hexatitanate whiskers and a solvent into a sealed homogenizing emulsifying machine for high-speed shearing and grinding to obtain premixed slurry, adding nano hollow glass beads and composite nano ceramic beads into the prepared premixed slurry, and continuously stirring and mixing to enable the controllable high-dispersion two-dimensional ultrathin titanium dioxide nanosheets, the nano hollow glass beads and the composite nano ceramic beads to be fully dispersed and uniformly mixed in the solvent, so as to obtain synthetic slurry;
(5) Adding the aqueous nano SiO 2 aerogel suspension emulsion, the synthetic slurry, the film forming auxiliary agent and the defoaming agent into the product obtained in the step (3), stirring at a low speed, dispersing uniformly to obtain the aqueous nano heat-preserving heat-insulating coating, and coating and drying to obtain the nano heat-preserving heat-insulating coating with the thickness of 2mm.
Example III
1) Preparation of controllable high-dispersion two-dimensional double-layer ultrathin titanium dioxide nanosheets
(1) Dissolving isopropyl titanate in a mixed solvent of glycol and deionized water, wherein the volume ratio of the glycol to deionized water is 2:1, magnetically stirring for 10min until the solution is uniformly mixed, transferring to a reaction kettle, reacting for 20h at 240 ℃, cooling to room temperature, washing with deionized water and an organic solvent for 5 times, and then placing in a vacuum drying oven for overnight drying at 120 ℃ to obtain dispersed titanium dioxide nanoclusters;
(2) Dispersing the titanium dioxide nanoclusters obtained in the step (1) in 150mL of buffer solution, and then adding dopamine hydrochloride into the buffer solution, wherein the mass ratio of the titanium dioxide nanoclusters to the dopamine hydrochloride is 5: and 1, magnetically stirring the suspension for 30 hours at room temperature, filtering, and calcining in a muffle furnace at the speed of 2 ℃/min for 3 hours at the temperature of 500 ℃ to finally obtain the controllable high-dispersion two-dimensional double-layer ultrathin titanium dioxide nanosheets.
2) Preparation of potassium hexatitanate whisker by nano-fiber template induced low-temperature heat treatment combined with flowing oxygen auxiliary thermal evaporation method
(1) Dissolving polyvinylidene fluoride in a mixed solvent of N, N-dimethylformamide and acetone, wherein the volume ratio of the N, N-dimethylformamide to the acetone is 3:1, heating the solution to 55 ℃ until polyvinylidene fluoride is completely dissolved;
(2) Adding potassium carbonate and titanium dioxide into the solution, continuously stirring to form a uniform solution, and preparing PVDF/(potassium carbonate and titanium dioxide) nanofiber felt by adopting an electrostatic spinning method under the voltage of 10 KV; the distance between the receiving plate and the spinning end is 15cm;
(3) Carrying out heat treatment on PVDF/(potassium carbonate and titanium dioxide) nanofiber felt at 180 ℃ for 12 hours through low-temperature treatment to obtain potassium hexatitanate crystal powder/PVDF nanofiber felt;
(4) In order to improve the formation of potassium hexatitanate whisker, pure O 2 is adopted as flowing atmosphere, the flow speed is 8L/min, a tube of aluminum oxide is heated to 750 ℃ in a muffle furnace, then the potassium hexatitanate crystal powder/PVDF nanofiber felt is placed in the tube of aluminum oxide to be sealed, the oxygen partial pressure is 60KPa, the tube is cooled to room temperature after being kept for 30min, and a potassium hexatitanate whisker sample is collected through a membrane filter placed between a vacuum tube and a vacuum pump.
3) Preparation of water-based nano heat-preservation heat-insulation coating
(1) Weighing the following raw materials in weight: 20 parts of solvent (the solvent is a combination of deionized water, ethanol or n-butanol, wherein the weight ratio is 10:5:5), 22 parts of methyl methacrylate weather-resistant emulsion, 10 parts of near infrared reflecting material bismuth molybdate, 10 parts of nano hollow glass beads, 10 parts of composite nano ceramic beads, 3.5 parts of SiO 2 aerogel, 3 parts of mica powder, 6 parts of potassium hexatitanate whisker, 10 parts of controllable high-dispersion two-dimensional ultrathin titanium dioxide nano sheet, 1 part of film forming auxiliary agent, 0.5 part of ultraviolet absorbent, 2 parts of flame retardant low-density magnesium hydroxide and 2 parts of stabilizer;
(2) Placing the methyl methacrylate emulsion and the SiO 2 aerogel into a sealed homogenizing emulsifying machine for stirring and mixing, so that the SiO 2 aerogel is fully dispersed, mixed and uniformly compounded in the emulsion to obtain a water-based nano SiO 2 aerogel suspension emulsion;
(3) Dispersing mica powder in a high-speed stirrer, and then placing near infrared reflecting material bismuth molybdate and flame retardant low-density magnesium hydroxide into the high-speed stirrer for continuous stirring until the materials are uniformly mixed;
(4) Loading the controllable high-dispersion two-dimensional ultrathin titanium dioxide nanosheets, potassium hexatitanate whiskers and a solvent into a sealed homogenizing emulsifying machine for high-speed shearing and grinding to obtain premixed slurry, adding nano hollow glass beads and composite nano ceramic beads into the prepared premixed slurry, and continuously stirring and mixing to enable the controllable high-dispersion two-dimensional ultrathin titanium dioxide nanosheets, the nano hollow glass beads and the composite nano ceramic beads to be fully dispersed and uniformly mixed in the solvent, so as to obtain synthetic slurry;
(5) Adding the aqueous nano SiO 2 aerogel suspension emulsion, the synthetic slurry, the film forming auxiliary agent and the defoaming agent into the product obtained in the step (3), stirring at a low speed, dispersing uniformly to obtain the aqueous nano heat-preserving heat-insulating coating, and coating and drying to obtain the nano heat-preserving heat-insulating coating with the thickness of 3mm.
As can be seen from fig. 4, the thickness of the coating layer is increased, the heat insulation performance is increased, but after a certain thickness is reached, the heat insulation performance is not increased or even slightly reduced, and the thickness is increased, so that the heat insulation performance is increased, probably because the thickness is increased, the electromagnetic waves which can penetrate through are fewer. When the thickness is reached, the light wave is difficult to penetrate, and the heat insulation performance of the light wave cannot be increased any more when the thickness is increased.
Table 1 Performance index of the aqueous nano thermal insulation coating of examples one, two and three

Claims (7)

1. The preparation method of the water-based nanometer heat preservation and heat insulation coating is characterized by comprising the following specific steps:
1) Preparation of controllable high-dispersion two-dimensional double-layer ultrathin titanium dioxide nanosheets
(1) Dissolving titanium salt in a mixed solvent of ethylene glycol and deionized water, magnetically stirring for 10-20 min until the solution is uniformly mixed, transferring into a reaction kettle, reacting for 20-24 h at 200-240 ℃, cooling to room temperature, washing with deionized water and an organic solvent for 3-5 times, and then placing in a vacuum drying oven for drying at 100-120 ℃ overnight to obtain dispersed titanium dioxide nanoclusters;
(2) Dispersing the titanium dioxide nanoclusters obtained in the step (1) in 100-150 mL of buffer solution, and then adding dopamine hydrochloride into the buffer solution, wherein the mass ratio of the titanium dioxide nanoclusters to the dopamine hydrochloride is (2-5): 1, magnetically stirring the suspension for 24-30 hours at room temperature, filtering, calcining in a muffle furnace at a speed of 1-2 ℃ per minute at 400-500 ℃ for 3-5 hours, and finally obtaining the controllable high-dispersion two-dimensional ultrathin titanium dioxide nanosheets;
2) Preparation of potassium hexatitanate whisker by nano-fiber template induced low-temperature heat treatment combined with flowing oxygen auxiliary thermal evaporation method
(1) Dissolving polyvinylidene fluoride in a mixed solvent of N, N-dimethylformamide and acetone, wherein the volume ratio of the N, N-dimethylformamide to the acetone is 1-3: 1, a step of; heating the solution to 50-55 ℃ until the polyvinylidene fluoride is completely dissolved;
(2) Adding potassium carbonate and titanium dioxide into the solution, continuously stirring to form a uniform solution, and preparing PVDF/(potassium carbonate and titanium dioxide) nanofiber felt by adopting an electrostatic spinning method under the voltage of 10-15 KV; the distance between the receiving plate and the spinning end is 10-15 cm;
(3) Carrying out low-temperature treatment on PVDF/(potassium carbonate and titanium dioxide) nanofiber felt at 140-180 ℃ for heat treatment
12-24 Hours to obtain potassium hexatitanate crystal powder/PVDF nanofiber felt;
(4) In order to improve the formation of potassium hexatitanate whisker, pure O2 is adopted as flowing atmosphere, the flow speed is 6-8L/min, a tube of aluminum oxide is heated to 600-750 ℃ in a muffle furnace, then potassium hexatitanate crystal powder/PVDF nanofiber felt is placed in the tube of aluminum oxide to be sealed, the oxygen partial pressure is 50-60 KPa, the tube is cooled to room temperature after being kept for 20-30 min, and a potassium hexatitanate whisker sample is collected through a membrane filter placed between a vacuum tube and a vacuum pump;
3) Preparation of water-based nano heat-preservation heat-insulation coating
(1) Weighing the following raw materials in weight: 20 parts of solvent, 22 parts of acrylic weather-resistant emulsion, 10 parts of near infrared reflecting material, 10 parts of nano hollow glass beads, 10 parts of composite nano ceramic beads, 3.5 parts of SiO2 aerogel, 3 parts of mica powder, 6 parts of potassium hexatitanate whisker, 10 parts of controllable high-dispersion two-dimensional ultrathin titanium dioxide nanosheets, 1 part of film forming auxiliary agent, 0.5 part of ultraviolet absorber, 2 parts of flame retardant and 2 parts of other auxiliary agents;
(2) Placing the acrylic emulsion and the SiO2 aerogel into a sealed homogenizing emulsifying machine for stirring and mixing, so that the SiO2 aerogel is fully dispersed, mixed and uniformly compounded in the emulsion to obtain a water-based nano SiO2 aerogel suspension emulsion;
(3) Dispersing mica powder in a high-speed stirrer, and then placing the near infrared reflecting material into the high-speed stirrer to continuously stir until the mica powder is uniformly mixed;
(4) Loading the controllable high-dispersion two-dimensional ultrathin titanium dioxide nanosheets, potassium hexatitanate whiskers and a solvent into a sealed homogenizing emulsifying machine for high-speed shearing and grinding to obtain premixed slurry, adding nano hollow glass beads and composite nano ceramic beads into the prepared premixed slurry, and continuously stirring and mixing to fully disperse the controllable high-dispersion two-dimensional ultrathin titanium dioxide nanosheets, the nano hollow glass beads and the composite nano ceramic beads in the solvent, and uniformly mixing to obtain synthetic slurry;
(5) Adding the aqueous nano SiO2 aerogel suspension emulsion, the synthetic slurry, the film forming auxiliary agent and other auxiliary agents into the product obtained in the step (3), stirring at a low speed, dispersing uniformly to obtain the aqueous nano heat-preserving heat-insulating coating, and coating and drying to obtain the nano heat-preserving heat-insulating coating.
2. The method for preparing the water-based nano heat-insulating coating according to claim 1, wherein the titanium salt is one or a combination of tetrabutyl titanate, isopropyl titanate and tetraisopropyl titanate.
3. The preparation method of the water-based nanometer heat preservation and heat insulation coating according to claim 1, which is characterized in that the volume ratio of the mixed solvent glycol to deionized water is 2-3: 1.
4. The method for preparing the water-based nano heat-preserving and heat-insulating coating according to claim 1, wherein the solvent is a combination of deionized water, ethanol and n-butanol, and the weight ratio is as follows: 10: 5-8: 2-5.
5. The method for preparing the water-based nano heat-preserving and heat-insulating coating according to claim 1, wherein the flame retardant is one or a combination of low-density magnesium hydroxide and aluminum hydroxide flame retardants.
6. The method for preparing the aqueous nano heat-preserving and heat-insulating coating according to claim 1, wherein the film-forming auxiliary agent is one or a combination of a defoaming agent, a leveling agent and a stabilizing agent.
7. The method for preparing the water-based nano heat-preserving and heat-insulating coating according to claim 1, wherein the near infrared reflecting material is one or a combination of indium tin oxide, sodium zinc phosphate and bismuth molybdate.
CN202210607606.6A 2022-05-31 2022-05-31 Preparation method of water-based nano heat-preservation heat-insulation coating Active CN115073981B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202210607606.6A CN115073981B (en) 2022-05-31 2022-05-31 Preparation method of water-based nano heat-preservation heat-insulation coating

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202210607606.6A CN115073981B (en) 2022-05-31 2022-05-31 Preparation method of water-based nano heat-preservation heat-insulation coating

Publications (2)

Publication Number Publication Date
CN115073981A CN115073981A (en) 2022-09-20
CN115073981B true CN115073981B (en) 2024-08-16

Family

ID=83249673

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202210607606.6A Active CN115073981B (en) 2022-05-31 2022-05-31 Preparation method of water-based nano heat-preservation heat-insulation coating

Country Status (1)

Country Link
CN (1) CN115073981B (en)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115445595A (en) * 2022-10-10 2022-12-09 国纳纳米技术研究(河北)有限公司 Preparation method of titanium dioxide nanosheet photocatalytic material, product and application thereof
CN115873427B (en) * 2022-10-10 2024-03-12 湖北兴瑞硅材料有限公司 Preparation method of silica aerogel/ceramic microbead composite hydrophobic heat-insulating coating
CN117887323B (en) * 2024-03-14 2024-06-25 浙江星辉新材料科技有限公司 Heat-reflecting coating composition, coating and heat-insulating felt and preparation methods thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106747265A (en) * 2016-12-27 2017-05-31 广州大学 A kind of aerogel composite and its preparation method based on self assembly opacifier fiber
CN109160777A (en) * 2018-10-22 2019-01-08 泉州臻美智能科技有限公司 A kind of fiber-reinforced composite heat-barrier material and preparation method thereof

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105086792A (en) * 2015-07-27 2015-11-25 北京恒固防腐工程有限公司 Environment-friendly waterborne nanometer constant-solid heat-preserving material and preparation method thereof
KR101847604B1 (en) * 2016-09-09 2018-04-11 주식회사 웨피 Aqueous, heat reflective, heat insulation and thermal insulation paint with excellent UV blocking capacity and method for production thereof
CN110054987A (en) * 2018-01-19 2019-07-26 北京泽马新技术有限公司 A kind of water nano thermal insulation paint
CN109437292A (en) * 2018-11-16 2019-03-08 大连理工大学 A kind of ultra-thin two-dimension titanium dioxide nanoplate efficiently synthesized and preparation method
CN109775757B (en) * 2019-03-19 2021-09-28 广州大学 Preparation method of three-dimensional titanium dioxide material
CN112521793A (en) * 2020-12-04 2021-03-19 廊坊森卓化工有限公司 Novel water-based nano heat-insulating coating and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106747265A (en) * 2016-12-27 2017-05-31 广州大学 A kind of aerogel composite and its preparation method based on self assembly opacifier fiber
CN109160777A (en) * 2018-10-22 2019-01-08 泉州臻美智能科技有限公司 A kind of fiber-reinforced composite heat-barrier material and preparation method thereof

Also Published As

Publication number Publication date
CN115073981A (en) 2022-09-20

Similar Documents

Publication Publication Date Title
CN115073981B (en) Preparation method of water-based nano heat-preservation heat-insulation coating
CN106700789B (en) Water-based building energy-saving coating and preparation method thereof
CN106752561A (en) A kind of aeroge compound heat-insulation coating and preparation method thereof
CN108658576B (en) Preparation method of composite silica aerogel felt
CN107267011A (en) A kind of coating with heat insulating reflecting function and preparation method thereof
CN107779024A (en) A kind of heat-preservation building paint containing nanoparticle and preparation method thereof
CN104844149A (en) Mullite fiber felt reinforced SiO2-Al2O3Preparation method of aerogel composite heat-insulating material
CN108249901B (en) Preparation method of high-temperature-resistant aerogel material
CN104108720B (en) A kind of preparation method of the silica aerogel particles of high daylight rate
CN101906261A (en) Thermal insulating glass coating with high leveling property
CN105295506A (en) Improved Stober method for preparing tio2/sio2 aerogel microsphere
CN114045071B (en) Building aluminum veneer curtain wall finish paint and preparation method thereof
CN108558344B (en) Preparation method of fireproof, waterproof and environment-friendly heat-preservation silicon aerogel paste
CN107057479A (en) A kind of aquosity heat insulating heat preserving fire proofing material and preparation method thereof
CN107674566B (en) Preparation method of hollow titanium dioxide @ silicon dioxide/waterborne polyurethane composite transparent heat-insulating coating
CN113801527A (en) Water-based transparent glass heat-insulating coating and preparation method thereof
CN109126643B (en) Self-light-modulation type transparent composite aerogel and preparation method thereof
CN103509462A (en) Heat insulation coating, preparation method and application thereof
Peng et al. High-efficiency energy-saving buildings utilizing potassium tungsten bronze heat-insulating glass and polyethylene glycol/expanded energy storage blanket
CN113372776B (en) Building sun-proof heat-insulating coating and preparation method thereof
CN102531536B (en) Flame retardant silica aerogel heat insulation composite material and preparation method thereof
CN111040623A (en) Special functional heat-insulation and temperature-reduction coating and preparation method thereof
CN111019445A (en) Special finish paint for reflective heat-insulating coating
CN112794334B (en) Aerogel type rare earth composite thermal insulation material and preparation method thereof
CN114181578A (en) External wall heat-preservation and heat-insulation composite building coating and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant