CN106634514A - Preparation method of hollow aluminum oxide ceramic microsphere modified polyurethane coating - Google Patents
Preparation method of hollow aluminum oxide ceramic microsphere modified polyurethane coating Download PDFInfo
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- CN106634514A CN106634514A CN201611194840.1A CN201611194840A CN106634514A CN 106634514 A CN106634514 A CN 106634514A CN 201611194840 A CN201611194840 A CN 201611194840A CN 106634514 A CN106634514 A CN 106634514A
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- preparation
- ceramic microsphere
- alumina ceramic
- hollow alumina
- coating
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Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
Abstract
The invention relates to a preparation method of a hollow aluminum oxide ceramic microsphere modified polyurethane coating. The preparation method comprises the following steps: preparing hollow aluminum oxide ceramic microspheres, namely treating aluminum nitrate and monosaccharide raw materials by virtue of steps of ultrasound, magnetic stirring, hydrothermal treatment, heat treatment and the like to obtain the hollow aluminum oxide ceramic microspheres with uniform particle size; and blending the obtained ceramic microspheres with waterborne polyurethane, and carrying out high-speed dispersion, ultrasound, spin coating and curing to obtain a composite coating. The preparation method provided by the invention has the advantages that nontoxic and easily available raw materials are adopted, a preparation process is simple, technology is controllable, cost is low, repeatability is good, and the hollow aluminum oxide ceramic microspheres are uniformly distributed. The prepared composite coating has the characteristics of environmental friendliness, light weight, high strength, high hardness, high wave transmission, low thermal conductivity, low infrared emissivity, excellent wear resistance, excellent weather resistance and the like and can be applied to the fields of heat insulation coatings, infrared stealth and the like.
Description
Technical field
The invention belongs to functional form composite coating technology field, is related to a kind of hollow alumina ceramic microsphere modified polyurethane
The preparation method of coating.
Background technology
In recent years, problems of energy consumption is severe all the more, and people increasingly increase the demand of energy-saving and emission-reduction material.Have concurrently heat-insulated
The multi-functional coatings of anti-wear performance can effectively reduce coating surface and internal temperature, in the extension device life-span, have ten to energy-saving
Divide important meaning.Multi-functional coatings are made up of film forming matter and functional filler.Film forming matter is made up of resin more, and tradition is molten
Formulation resin includes a large amount of volatilizable organic compounds, endangers environment and resistance to water is poor, significantly limit its application.Oxidation
The functional fillers such as aluminium flake, titanium dioxide, silica, zinc oxide enhance to a certain extent the intensity of coating, hardness, resistance to
Mill, etc. mechanical property and give the characteristics such as the heat-insulated, antibacterial of coating.But it is light that the shortcomings of its density height, lack of homogeneity, limits coating
The application of matter and development.
Document 1 " department takes charge of great courage from brightness, and Chen An is congruent. a kind of nanometer alumina modified acrylic resin type powdery paints,
China, CN104945972B.2014 " is disclosed and a kind of prepared the aluminum oxide with excellent adhesive attraction, weatherability, corrosion resistance and change
The method of property acrylic resin type powdery paints.But, the method with solid alumina as functional filler, gained coating density
It is larger and production process is complicated, it is wayward.
Document 2 " Wang Fangfang, Guo Hanyu, Li Ji. the preparation of organic-inorganic compoiste nano heat-insulating fireproof coating and performance
Research [J]. architecture science, 2015,31:24-28. " discloses one kind and prepares organic-inorganic compoiste nano heat-insulating fireproof coating
Method.The coating is compound as organic binder, nanometer hydrogen-oxygen using water-and acrylate emulsion and aqueous epoxy resin emulsion
Change the heat-insulating, fire-preventing coating that aluminium, ceramic hollow microballon, titanium dioxide etc. prepare excellent performance for inorganic filler.But, gained
Coating can decompose generation H under heated environment2O, forms pore, accelerates the failure of coating mechanical property.
It can be seen that：The shortcomings of there is pollution environment, poor water resistance, higher density in traditional solvent-borne polyurethane based coatings
The content of the invention
The technical problem to be solved
In order to avoid the deficiencies in the prior art part, the present invention proposes a kind of hollow alumina ceramic microsphere modified polyurethane
The preparation method of coating, with aqueous polyurethane as film forming matter, hollow alumina Ceramic Balls are functional filler to the composite coating.
The method has the advantages that preparation process is simple, with low cost, reaction are controllable.
Technical scheme
A kind of preparation method of hollow alumina ceramic microsphere modified polyurethane coating, it is characterised in that step is as follows：
Step 1：By Al (NO3)3·9H2(2～4) ︰ (20～40) mix O ︰ mono- Tang ︰ deionized waters 1 ︰ in mass ratio, ultrasound
Process and obtain homogeneous solution with after magnetic agitation；Resulting solution is placed in ptfe autoclave inner bag, 150～220
2～24h is incubated at a temperature of DEG C, brown gel liquid is obtained；Adopt and be washed with deionized brown gel liquid and be to pH value
7, vacuum filtration obtains solid sample, and 8～40h is dried under 40～80 DEG C of vacuum conditions；
Step 2：Step 1 is dried into product to be placed in alumina crucible, in air atmosphere, it is hot in 1200～1500 DEG C at
1～10h of reason, obtains hollow alumina ceramic microsphere；Gained hollow alumina ceramic microsphere particle diameter is 0.1～5 μm.
Step 3：By the grinding of hollow alumina ceramic microsphere, carry out altogether by 1～50wt% of mass fraction and aqueous polyurethane
It is mixed, disperse 0.1～1.5h, 10～120min of ultrasonic disperse under 3000～6000rpm rotating speeds at a high speed, obtain uniform dispersion；Will
Homogeneous dispersion is applied on circular slide, and spin coating is carried out with spin coater, obtains wet film in uniform thickness；The spin coating parameters
It is as follows：500～1000r/min of low speed, 10～30s of time；1600～2000r/min, 5～60s of time at a high speed；
Step 4：Gained wet film is solidified under 40～80 DEG C of vacuum conditions 0.5～4h；Weight on slide after hardening
Multiple above-mentioned steps, obtain the hollow alumina ceramic microsphere/aqueous polyurethane composite coating of different-thickness.Used film forming material is
Aqueous polyurethane.
The ultrasonically treated of the step 2 is 10～60min.
The magnetic agitation of the step 2 is 10～60min.
The monose can be fructose or glucose.
Beneficial effect
The preparation method of a kind of hollow alumina ceramic microsphere modified polyurethane coating proposed by the present invention, by hollow oxidation
Aluminium ceramic microsphere is compounded to form coating with aqueous polyurethane.Aqueous polyurethane with water as solvent, with environmentally friendly, nontoxic, compatibility
Well, the advantages of intensity height, good toughness, superior abrasion resistance, traditional solvent-borne resin poor water resistance, pollution environment etc. are overcome and is lacked
Point, becomes the study hotspot of following coatings art.Hollow alumina ceramic microsphere has high intensity, high rigidity, thermal coefficient of expansion
The good physical-chemical performances such as little, anti-thermal shock, shrinkage factor are low, wear-resisting, corrosion-resistant, wave transparent and low infrared emission.
Hollow alumina ceramic microsphere modified polyurethane coating prepared by the present invention, overcomes solvent type resin pollution ring
Border, the shortcoming of poor water resistance, enhance intensity, hardness, wearability, the weatherability of coating.Additionally, hollow alumina ceramic microsphere
The properties such as low infrared emissivity, lower thermal conductivity, high wave transmission rate have widened application of the coating in the field such as heat-insulated and electromagnetic wave is stealthy.
The method of the composite coating with premium properties such as environmental protection, light weight, heat-insulated, wear-resisting, corrosion-resistant, wave transparent, low infrared emissions.This is answered
Coating is closed with aqueous polyurethane as film forming matter, hollow alumina Ceramic Balls are functional filler.The method has preparation technology
Simply, it is with low cost, react it is controllable the advantages of.
Description of the drawings
Fig. 1 is the process chart of the inventive method
Specific embodiment
In conjunction with embodiment, accompanying drawing, the invention will be further described：
Embodiment one
The present embodiment is comprised the following steps：
Weigh 2gAl (NO3)3·9H2O, 5g glucose, in being added to 70ml deionized waters, ultrasonic 10min, magnetic agitation
10min, in inserting 100ml ptfe autoclaves, at 160 DEG C 24h is incubated；By gained brown liquid as a form of gel spend from
Sub- water washing to solution ph is about 7, and 24h is vacuum dried at 80 DEG C after vacuum filtration；Products therefrom is put into into high-temperature tubular
Stove, 1200 DEG C of sintering 2h, that is, obtain hollow alumina ceramic microsphere.
Take 0.01g hollow alumina ceramic microspheres to be added in 3.3g aqueous polyurethane coatings (solid content 30%),
Disperse 1.5h, ultrasonic disperse 0.5h under 6000rpm rotating speeds at a high speed.Gained dispersion liquid is carried out into film with spin coater, spin coater is low
Fast 600r/min, time 30s, high speed 1800r/min, time 20s；Gained wet film is put in vacuum drying chamber, it is true at 80 DEG C
Sky is dried 0.5h, that is, obtain hollow alumina ceramic microsphere/aqueous polyurethane composite coating.
Embodiment two
The present embodiment is comprised the following steps：
Weigh 1gAl (NO3)3·9H2O, 3g fructose mixes, and in being added to 70ml deionized waters, ultrasonic 20min, magnetic force is stirred
20min is mixed, in inserting 100ml ptfe autoclaves, at 180 DEG C 22h is incubated；Gained brown liquid as a form of gel is spent
Ion water washing to solution ph is about 7, and 24h is vacuum dried at 80 DEG C after vacuum filtration；Products therefrom is put into into high temperature pipe
Formula stove, 1300 DEG C of sintering 5h, that is, obtain hollow alumina ceramic microsphere.
Take 0.1g hollow alumina ceramic microspheres to be added in 3.3g aqueous polyurethane coatings (solid content 30%),
Disperse 1.5h, ultrasonic disperse 0.1h under 3000rpm rotating speeds at a high speed.Gained dispersion liquid is carried out into film with spin coater, spin coater is low
Fast 500r/min, time 30s, high speed 2000r/min, time 20s；Gained wet film is put in vacuum drying chamber, it is true at 40 DEG C
Sky is dried 4h, that is, obtain hollow alumina ceramic microsphere/aqueous polyurethane composite coating.
Embodiment three
The present embodiment is comprised the following steps：
(1) 4gAl (NO are weighed3)3·9H2O, 10g fructose mixes, in being added to 70ml deionized waters, ultrasonic 60min, and magnetic
Power stirs 60min, in inserting 100ml ptfe autoclaves, at 220 DEG C 2h is incubated；By gained brown liquid as a form of gel
It is washed with deionized to solution ph and is about 7,24h is vacuum dried at 80 DEG C after vacuum filtration；Products therefrom is put into into height
Warm tube furnace, 1500 DEG C of sintering 1h, that is, obtain hollow alumina ceramic microsphere.
(2) take 0.5g hollow alumina ceramic microspheres to be added in 3.3g aqueous polyurethane coatings (solid content 30%),
Disperse 1h, ultrasonic disperse 1h under 6000rpm rotating speeds at a high speed.Gained dispersion liquid is carried out into film, spin coater low speed with spin coater
800r/min, time 20s, high speed 2000r/min, time 5s；Gained wet film is put in vacuum drying chamber, vacuum is done at 40 DEG C
Dry 4h, that is, obtain hollow alumina ceramic microsphere/aqueous polyurethane composite coating.
Embodiment four
The present embodiment is comprised the following steps：
(1) 2gAl (NO are weighed3)3·9H2O, 5g fructose mixes, in being added to 70ml deionized waters, ultrasonic 30min, and magnetic force
Stirring 30min, in inserting 100ml ptfe autoclaves, at 200 DEG C 18h is incubated；Gained brown liquid as a form of gel is used
Deionized water is washed to solution ph and is about 7, and 18h is vacuum dried at 60 DEG C after vacuum filtration；Products therefrom is put into into high temperature
Tube furnace, 1400 DEG C of sintering 1h, that is, obtain hollow alumina ceramic microsphere.
(2) take 1g hollow alumina ceramic microspheres to be added in 3.3g aqueous polyurethane coatings (solid content 30%),
Disperse 0.1h, ultrasonic disperse 2h under 4500rpm rotating speeds at a high speed.Gained dispersion liquid is carried out into film, spin coater low speed with spin coater
1000r/min, time 10s, high speed 2000r/min, time 60s；Gained wet film is put in vacuum drying chamber, vacuum at 40 DEG C
4h is dried, that is, obtains hollow alumina ceramic microsphere/aqueous polyurethane composite coating.
Claims (4)
1. a kind of preparation method of hollow alumina ceramic microsphere modified polyurethane coating, it is characterised in that step is as follows：
Step 1：By Al (NO3)3·9H2(2～4) ︰ (20～40) mix O ︰ mono- Tang ︰ deionized waters 1 ︰ in mass ratio, ultrasonically treated
With homogeneous solution is obtained after magnetic agitation；Resulting solution is placed in ptfe autoclave inner bag, in 150～220 DEG C of temperature
Degree 2～24h of lower insulation, obtains brown gel liquid；It is 7 to adopt and be washed with deionized brown gel liquid to pH value, very
Empty suction filtration obtains solid sample, and 8～40h is dried under 40～80 DEG C of vacuum conditions；
Step 2：Step 1 is dried into product to be placed in alumina crucible, in air atmosphere, in 1200～1500 DEG C 1 is heat-treated
～10h, obtains hollow alumina ceramic microsphere；
Step 3：By the grinding of hollow alumina ceramic microsphere, it is blended with aqueous polyurethane by 1～50wt% of mass fraction,
Disperse 0.1～1.5h, 10～120min of ultrasonic disperse under 3000～6000rpm rotating speeds at a high speed, obtain uniform dispersion；Will dispersion
Liquid uniform application carries out spin coating with spin coater on circular slide, obtains wet film in uniform thickness；The spin coating parameters are such as
Under：500～1000r/min of low speed, 10～30s of time；1600～2000r/min, 5～60s of time at a high speed；
Step 4：Gained wet film is solidified under 40～80 DEG C of vacuum conditions 0.5～4h；On repeating on slide after hardening
Step is stated, the hollow alumina ceramic microsphere/aqueous polyurethane composite coating of different-thickness is obtained.
2. the preparation method of hollow alumina ceramic microsphere modified polyurethane coating according to claim 1, it is characterised in that：
The ultrasonically treated of the step 2 is 10～60min.
3. the preparation method of hollow alumina ceramic microsphere modified polyurethane coating according to claim 1, it is characterised in that：
The magnetic agitation of the step 2 is 10～60min.
4. the preparation method of hollow alumina ceramic microsphere modified polyurethane coating according to claim 1, it is characterised in that：
The monose can be fructose or glucose.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108948719A (en) * | 2018-06-12 | 2018-12-07 | 安徽喜宝高分子材料有限公司 | A kind of heat-insulated counnter attack optical thin film of instrument desk and preparation method thereof |
| RU2740748C1 (en) * | 2020-04-03 | 2021-01-20 | Федеральное государственное бюджетное учреждение науки Физико-технологический институт им. А.Ф. Иоффе Российской академии наук | Method of producing hollow microspheres of aluminium oxide |
| CN112876900A (en) * | 2021-02-05 | 2021-06-01 | 江南大学 | Method for reducing shrinkage stress of thermal curing coating by using hollow microspheres |
| CN114907754A (en) * | 2021-02-09 | 2022-08-16 | 马自达汽车株式会社 | Coating material and method for coating resin molded article using the same |
| CN115851096A (en) * | 2022-12-16 | 2023-03-28 | 苏州鸿钜金属制品有限公司 | Flame-retardant insulating coating based on coated hollow alumina and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108948719A (en) * | 2018-06-12 | 2018-12-07 | 安徽喜宝高分子材料有限公司 | A kind of heat-insulated counnter attack optical thin film of instrument desk and preparation method thereof |
| RU2740748C1 (en) * | 2020-04-03 | 2021-01-20 | Федеральное государственное бюджетное учреждение науки Физико-технологический институт им. А.Ф. Иоффе Российской академии наук | Method of producing hollow microspheres of aluminium oxide |
| CN112876900A (en) * | 2021-02-05 | 2021-06-01 | 江南大学 | Method for reducing shrinkage stress of thermal curing coating by using hollow microspheres |
| CN112876900B (en) * | 2021-02-05 | 2021-11-05 | 江南大学 | Method for reducing shrinkage stress of thermal curing coating by using hollow microspheres |
| CN114907754A (en) * | 2021-02-09 | 2022-08-16 | 马自达汽车株式会社 | Coating material and method for coating resin molded article using the same |
| CN115851096A (en) * | 2022-12-16 | 2023-03-28 | 苏州鸿钜金属制品有限公司 | Flame-retardant insulating coating based on coated hollow alumina and preparation method thereof |
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Application publication date: 20170510 |