CN109266206A - A kind of preparation method of nanometer heat isolation paint - Google Patents
A kind of preparation method of nanometer heat isolation paint Download PDFInfo
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- CN109266206A CN109266206A CN201811104015.7A CN201811104015A CN109266206A CN 109266206 A CN109266206 A CN 109266206A CN 201811104015 A CN201811104015 A CN 201811104015A CN 109266206 A CN109266206 A CN 109266206A
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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
- C09D175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/66—Additives characterised by particle size
- C09D7/67—Particle size smaller than 100 nm
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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
- 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
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- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/262—Alkali metal carbonates
Abstract
The invention discloses a kind of preparation methods of nanometer heat isolation paint, belong to macromolecule heat-barrier material technical field.According to parts by weight, it successively weighs: 30~40 parts of polyurethane acroleic acids, 10~15 portions of reactive diluents, 5~10 parts of photoinitiators, 3~5 parts of levelling agents, 2~6 parts of wetting agent BYK, 2~8 parts of dispersing agents, 50~60 parts of mixed solvents and 20~25 parts of additives；Polyurethane acroleic acid is mixed with mixed solvent, and sequentially adds reactive diluent, photoinitiator, levelling agent, wetting agent BYK, dispersing agent and additive after being stirred, obtain nanometer heat isolation paint.The nanometer heat isolation paint of technical solution of the present invention preparation has the characteristics that excellent heat-proof quality and wear-resisting property, has broad prospects in the development of macromolecule heat-barrier material technology industry.
Description
Technical field
The invention discloses a kind of preparation methods of nanometer heat isolation paint, belong to macromolecule heat-barrier material technical field.
Background technique
Most important component first is that thermal insulating filling in insulating moulding coating.(such as hollow glass, ceramics are micro- for common thermal insulating filling
Pearl etc.) belong to high interstitital texture material, these filler heat shieldings are good, the microcellular structure that can increase coating or the shape in coating
At stable thermal insulation layer to realize the heat-insulated of coating, they have, and thermal coefficient is small, small (less quality is with regard to reachable for bulk density
To preferable heat insulation), surface area it is small, weatherability, the features such as corrosion resistance is strong, therefore obtained extensively in insulating moulding coating field
Using.However, constructional difficulties thicker by the usual film of insulating moulding coating prepared by this kind of filler, to some high-tech such as military project, boat
Empty space industry etc. is simultaneously not suitable for, and heat insulation is undesirable, it is therefore necessary to develop the better coating of heat insulation to substitute
Traditional insulating moulding coating.In recent years, a large amount of nano material is used for the exploitation of insulating moulding coating.With traditional thermal insulating filling phase
Than the maximum difference of nano material is its skin effect, dimensional effect, quantum effect and bulk effect, is added into coating
In in addition to it can improve to film performance, can also assign film special function.Effect of the nano material for insulating moulding coating
It is mainly reflected in several aspects: 1. enhancing the physical property of film, improve hardness, wear resistance of film etc.；2. improving film
Weatherability, corrosion resistance, the performances such as ageing-resistant, anti-radiation；3. changing coating structure, increase the porosity in coating；4. benefit
With the characteristic of certain nanoparticles, the barrier to heat is realized.There are many type of nano material, the heat-insulated machine of nanometer heat isolation paint
Reason is also not quite similar, even if the identical insulating moulding coating of insulating mechanism, heat insulation also can be with the dosage and ratio of thermal insulating filling
Example and change.Other than the physical properties such as hardness, wear resistance of influence of the nano material to thermal barrier coating in addition to enhancing coating,
For improving the thermodynamic property of coating, the thermal conductivity for such as reducing coating, the coefficient of thermal expansion for increasing coating, enhancing coating are followed in heat
Thermal shock resistance etc. under ring also has remarkable effect.Firstly, after high-temperature heat treatment, nanoparticle depositing in the coating
There are 2 kinds in form, a portion nanoparticle increases by fusing recrystallization, partial size；Another part particle does not melt then,
Maintain original crystallite dimension and grain structure.Without the nanoparticle of fusing
Son is loosely distributed in the nanoparticle of fusing, and after coating is cooling, thermal stress relaxation can between these nanoparticles
Generate a large amount of micron orders or nanoscale hole.
And traditional nanometer heat isolation paint the problem of can not further being promoted there is also heat-proof quality and wear-resisting property, because
This, the shortcomings that how improving Conventional nano insulating moulding coating, develops the nano heat-insulating with good comprehensive performance and applies in the hope of exploring
Material is problem to be solved.
Summary of the invention
The present invention solves the technical problem of: it can not for Conventional nano heat-insulation property of heat-insulation coating and wear-resisting property
The shortcomings that further being promoted provides a kind of preparation method of nanometer heat isolation paint.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
A kind of preparation method of nanometer heat isolation paint, specific preparation step are as follows:
(1) by potassium carbonate, 1.2:4.0~1.5:4.0 is mixed in molar ratio with titanium dioxide, grinding, high temperature sintering, and discharging is washed
It washs, dry, grinding obtains mixed-powder；
(2) mixed-powder is mixed with ethanol solution 1:30~1:60 in mass ratio, and mixed-powder quality 0.2~0.3 is added
Times polyallylamine hydrochlorides, after being stirred, obtain polyallylamine hydrochlorides mixture, by polyallylamine hydrochlorides mixture with
Stannic chloride 8:1~10:1 in mass ratio mixing, and be added 0.1~0.2 times of stannic chloride quality lead chloride and stannic chloride quality 3~
5 times of butyl titanate after being stirred, adjusts pH to 8~10, stands, filters, dry, obtains pre- modified powder；
(3) pre- modified powder is calcined, obtains modified powder, modified powder and graphene oxide 1:1~2:1 in mass ratio are mixed
It closes, and 15~30 times of modified powder quality of trishydroxymethylaminomethane buffer solution is added, after ultrasonic disperse, obtain modified powder
Mixture mixes modified powder mixture with dopamine 15:2~18:2 in mass ratio, after being stirred to react, filters, dry, obtains
Additive；
(4) according to parts by weight, it successively weighs: 30~40 parts of polyurethane acroleic acids, 10~15 portions of reactive diluents, 5~10 parts
Photoinitiator, 3~5 parts of levelling agents, 2~6 parts of wetting agent BYK, 2~8 parts of dispersing agents, 50~60 parts of mixed solvents and 20~25 parts
Additive；Polyurethane acroleic acid is mixed with mixed solvent, and sequentially adds reactive diluent, photoinitiator, levelling agent, wetting
Agent BYK, dispersing agent and additive after being stirred, obtain nanometer heat isolation paint.
Step (1) high temperature sintering is to be warming up to 700~850 DEG C with the heating rate of 5~10 DEG C/min, heat preservation sintering
12~14h.
Step (3) calcination temperature is 700~750 DEG C.
Step (3) the trishydroxymethylaminomethane buffer solution is by trishydroxymethylaminomethane and water in mass ratio 1:
80~1:90 mixing, adjusts pH to 8.0~8.5, obtains trishydroxymethylaminomethane buffer solution.
Step (4) reactive diluent is reactive diluent HK-66, reactive diluent HELOXY61 or reactive diluent
Any one in HELOXY62.
Step (4) photoinitiator is photoinitiator TPO, any one in photoinitiator 184 or photoinitiator 907.
Step (4) levelling agent is any one in silicone oil or dimethyl silicone polymer.
Step (4) dispersing agent is dispersing agent NNO, any one in Dispersant MF or dispersing agent 5040.
Step (4) mixed solvent is to mix ethyl acetate with butyl acetate 1:1~3:1 in mass ratio, must be mixed
Solvent.
The beneficial effects of the present invention are:
Additive is added when preparing nanometer heat isolation paint by the present invention, firstly, containing the lamellar structure of potassium tetratitanate in additive,
Thermal coefficient is smaller, after being added in product, can reduce heat radiation suffered by product, so that the heat-proof quality of product is improved,
Also, due to the presence of lamellar structure, to be the wearability raising of product, secondly as the lamellar structure of potassium tetratitanate has
There is ion-exchange capacity, it, can deposition of titanium oxide and antimony oxide in the lamellar structure of potassium tetratitanate in additive preparation process
Tin, and under the action of polyallylamine hydrochlorides, so that titanium dioxide and antimony tin is present in lamellar structure with nano-form
In, since titanium dioxide and antimony tin have preferable heat radiation reflecting properties, to be worn in potassium tetratitanate lamellar structure
Afterwards, making product still has preferable heat-proof quality, so that the service life of product be made to improve, heat-proof quality is further increased, then
Person, additive makes potassium tetratitanate be carried on graphene surface during the preparation process, and graphene has dopamine oxygen reduction fossil
Black alkene is made, on the one hand, the graphene of addition can further improve the wear-resisting property of product, on the other hand, be restored with dopamine
The dispersibility of graphene can be improved in graphene made from graphene oxide, to improve the dispersibility of additive in the product, makes
The heat-proof quality of product further increases, and due to the bonding force of dopamine, the binding force between graphene and matrix can be improved,
And then further increase the wearability of product.
Specific embodiment
Trishydroxymethylaminomethane is mixed with water 1:80~1:90 in mass ratio, the hydrochloric acid for being 8~10% with mass fraction
The pH to 8.0~8.5 for adjusting trishydroxymethylaminomethane and aqueous mixtures, obtains trishydroxymethylaminomethane buffer solution；By carbon
1.2:4.0~1.5:4.0 is mixed in grinder sour potassium in molar ratio with titanium dioxide, after 1~2h of mixed grinding, obtains mixed powder
Last blank, by mixed-powder blank high temperature sintering, discharging obtains pretreatment mixed-powder, by pretreatment mixed powder first with quality point
After number is salt acid elution 5~8 times of 12~15%, then it is washed with deionized, and by the pretreatment mixed powder after washing in temperature
Under conditions of being 70~80 DEG C after dry 2~5h, mixed-powder is obtained；The ethyl alcohol for being 50~60% by mixed-powder and mass fraction
Solution 1:30~1:60 in mass ratio is mixed in beaker, and 0.2~0.3 times of mixed-powder quality of polyene is added into beaker
Propylamin hydrochloride is 30~40 DEG C in temperature, under conditions of revolving speed is 500~600r/min, after being stirred 1~3h, obtains poly-
Polyallylamine hydrochlorides mixture and stannic chloride 8:1~10:1 in mass ratio are mixed in flask by allylamine hydrochloride mixture
In, and 0.1~0.2 times of stannic chloride quality of lead chloride and 3~5 times of stannic chloride quality of butyl titanate are added into flask,
In temperature be 45~60 DEG C, revolving speed be 300~450r/min under conditions of, after being stirred 1~2h, with mass fraction be 10~
15% ammonium hydroxide adjusts the pH to 8~10 of material in flask, and after standing 10~12h under room temperature, and filtering obtains filter cake, will
Under conditions of filter cake is 60~80 DEG C in temperature after dry 1~3h, pre- modified powder is obtained；Pre- modified powder is moved into Muffle furnace
After calcining 1~3h, Muffle in-furnace temperature is down to room temperature, discharges, obtains modified powder, modified powder and graphene oxide are pressed into matter
Amount is mixed in three-necked flask than 1:1~2:1, and 15~30 times of modified powder quality of trihydroxy methyl is added into three-necked flask
Aminomethane buffer solution obtains modified powder mixing under conditions of frequency is 45~55kHz after 30~50min of ultrasonic disperse
Object mixes modified powder mixture with dopamine 15:2~18:2 in mass ratio, in temperature be 60 DEG C, revolving speed be 600~
Under conditions of 800r/min, be stirred to react 20~for 24 hours after, filtering obtains additive blank, by additive blank in temperature be 70~
Under conditions of 80 DEG C after dry 50~80min, additive is obtained；According to parts by weight, it successively weighs: 30~40 parts of polyurethane propylene
Acid, 10~15 portions of reactive diluents, 5~10 parts of photoinitiators, 3~5 parts of levelling agents, 2~6 parts of wetting agent BYK, 2~8 parts of dispersions
Agent, 50~60 parts of mixed solvents and 20~25 parts of additives；Polyurethane acroleic acid and mixed solvent are mixed in blender, and
Reactive diluent, photoinitiator, levelling agent, wetting agent BYK, dispersing agent and additive are successively added into blender, in temperature
It is 30~50 DEG C, under conditions of revolving speed is 300~500r/min, after being stirred 1~2h, obtains nanometer heat isolation paint.The height
Temperature, which is sintered to, is warming up to 700~850 DEG C with the heating rate of 5~10 DEG C/min, 12~14h of heat preservation sintering.The calcination temperature
It is 700~750 DEG C.The reactive diluent is reactive diluent HK-66, reactive diluent HELOXY61 or reactive diluent
Any one in HELOXY62.The photoinitiator is photoinitiator TPO, any one in photoinitiator 184 or photoinitiator 907
Kind.The levelling agent is any one in silicone oil or dimethyl silicone polymer.The dispersing agent is dispersing agent NNO, Dispersant MF
Or any one in dispersing agent 5040.The mixed solvent is to mix ethyl acetate and butyl acetate 1:1~3:1 in mass ratio
It closes, obtains mixed solvent.
Trishydroxymethylaminomethane is mixed with water 1:90 in mass ratio, adjusts three hydroxyls with the hydrochloric acid that mass fraction is 10%
The pH to 8.5 of aminomethane and aqueous mixtures, obtains trishydroxymethylaminomethane buffer solution；By potassium carbonate and titanium dioxide
1.5:4.0 is mixed in grinder in molar ratio, after mixed grinding 2h, obtains mixed-powder blank, by mixed-powder blank high temperature
Sintering, discharging, obtains pretreatment mixed-powder, mixed powder will be pre-processed and first use mass fraction be 15% salt acid elution for 8 times after, then
Be washed with deionized, and by the pretreatment mixed powder after washing be 80 DEG C in temperature under conditions of after dry 5h, obtain mixed powder
End；The ethanol solution 1:60 in mass ratio that mixed-powder and mass fraction are 60% is mixed in beaker, and is added into beaker
The polyallylamine hydrochlorides that 0.3 times of mixed-powder quality are 40 DEG C in temperature, and under conditions of revolving speed is 600r/min, stirring is mixed
After closing 3h, polyallylamine hydrochlorides mixture is obtained, polyallylamine hydrochlorides mixture is mixed with stannic chloride 10:1 in mass ratio
In flask, and 0.2 times of stannic chloride quality of lead chloride and 5 times of stannic chloride quality of butyl titanate are added into flask, in
Temperature is 60 DEG C, under conditions of revolving speed is 450r/min, after being stirred 2h, adjusts flask with the ammonium hydroxide that mass fraction is 15%
The pH to 10 of interior material, and after standing 12h under room temperature, filtering obtains filter cake, by filter cake under conditions of temperature is 80 DEG C
After dry 3h, pre- modified powder is obtained；Pre- modified powder is moved into Muffle furnace after calcining 3h, Muffle in-furnace temperature is down to room
Temperature, discharging, obtains modified powder, modified powder and graphene oxide 2:1 in mass ratio is mixed in three-necked flask, and to three mouthfuls
30 times of modified powder quality of trishydroxymethylaminomethane buffer solution is added in flask, surpasses under conditions of frequency is 55kHz
After sound disperses 50min, modified powder mixture is obtained, modified powder mixture is mixed with dopamine 18:2 in mass ratio, Yu Wen
Degree is 60 DEG C, and under conditions of revolving speed is 800r/min, after being stirred to react for 24 hours, filtering obtains additive blank, by additive blank
Under conditions of being 80 DEG C in temperature after dry 80min, additive is obtained；According to parts by weight, it successively weighs: 40 parts of polyurethane propylene
Acid, 15 portions of reactive diluents, 10 parts of photoinitiators, 5 parts of levelling agents, 6 parts of wetting agent BYK, 8 parts of dispersing agents, 60 parts of mixed solvents
With 25 parts of additives；Polyurethane acroleic acid and mixed solvent are mixed in blender, and activity is successively added into blender
Diluent, photoinitiator, levelling agent, wetting agent BYK, dispersing agent and additive are 50 DEG C in temperature, and revolving speed is 500r/min's
Under the conditions of, after being stirred 2h, obtain nanometer heat isolation paint.The high temperature sintering is to be warming up to the heating rate of 10 DEG C/min
850 DEG C, heat preservation sintering 14h.The calcination temperature is 750 DEG C.The reactive diluent is reactive diluent HK-66.The light
Initiator is photoinitiator TPO.The levelling agent is silicone oil.The dispersing agent is dispersing agent NNO.The mixed solvent is by second
Acetoacetic ester is mixed with butyl acetate 3:1 in mass ratio, obtains mixed solvent.
Trishydroxymethylaminomethane is mixed with water 1:90 in mass ratio, adjusts three hydroxyls with the hydrochloric acid that mass fraction is 10%
The pH to 8.5 of aminomethane and aqueous mixtures, obtains trishydroxymethylaminomethane buffer solution；By potassium carbonate and titanium dioxide
1.5:4.0 is mixed in grinder in molar ratio, after mixed grinding 2h, obtains mixed-powder blank, by mixed-powder blank high temperature
Sintering, discharging, obtains pretreatment mixed-powder, mixed powder will be pre-processed and first use mass fraction be 15% salt acid elution for 8 times after, then
Be washed with deionized, and by the pretreatment mixed powder after washing be 80 DEG C in temperature under conditions of after dry 5h, obtain mixed powder
End；The ethanol solution 1:60 in mass ratio that mixed-powder and mass fraction are 60% is mixed in beaker, in temperature be 40 DEG C,
Under conditions of revolving speed is 600r/min, after being stirred 3h, mixture is obtained, mixture is mixed with stannic chloride 10:1 in mass ratio
In flask, and 0.2 times of stannic chloride quality of lead chloride and 5 times of stannic chloride quality of butyl titanate are added into flask, in
Temperature is 60 DEG C, under conditions of revolving speed is 450r/min, after being stirred 2h, adjusts flask with the ammonium hydroxide that mass fraction is 15%
The pH to 10 of interior material, and after standing 12h under room temperature, filtering obtains filter cake, by filter cake under conditions of temperature is 80 DEG C
After dry 3h, pre- modified powder is obtained；Pre- modified powder is moved into Muffle furnace after calcining 3h, Muffle in-furnace temperature is down to room
Temperature, discharging, obtains modified powder, modified powder and graphene oxide 2:1 in mass ratio is mixed in three-necked flask, and to three mouthfuls
30 times of modified powder quality of trishydroxymethylaminomethane buffer solution is added in flask, surpasses under conditions of frequency is 55kHz
After sound disperses 50min, modified powder mixture is obtained, modified powder mixture is mixed with dopamine 18:2 in mass ratio, Yu Wen
Degree is 60 DEG C, and under conditions of revolving speed is 800r/min, after being stirred to react for 24 hours, filtering obtains additive blank, by additive blank
Under conditions of being 80 DEG C in temperature after dry 80min, additive is obtained；According to parts by weight, it successively weighs: 40 parts of polyurethane propylene
Acid, 15 portions of reactive diluents, 10 parts of photoinitiators, 5 parts of levelling agents, 6 parts of wetting agent BYK, 8 parts of dispersing agents, 60 parts of mixed solvents
With 25 parts of additives；Polyurethane acroleic acid and mixed solvent are mixed in blender, and activity is successively added into blender
Diluent, photoinitiator, levelling agent, wetting agent BYK, dispersing agent and additive are 50 DEG C in temperature, and revolving speed is 500r/min's
Under the conditions of, after being stirred 2h, obtain nanometer heat isolation paint.The high temperature sintering is to be warming up to the heating rate of 10 DEG C/min
850 DEG C, heat preservation sintering 14h.The calcination temperature is 750 DEG C.The reactive diluent is reactive diluent HK-66.The light
Initiator is photoinitiator TPO.The levelling agent is silicone oil.The dispersing agent is dispersing agent NNO.The mixed solvent is by second
Acetoacetic ester is mixed with butyl acetate 3:1 in mass ratio, obtains mixed solvent.
Trishydroxymethylaminomethane is mixed with water 1:90 in mass ratio, adjusts three hydroxyls with the hydrochloric acid that mass fraction is 10%
The pH to 8.5 of aminomethane and aqueous mixtures, obtains trishydroxymethylaminomethane buffer solution；By potassium carbonate and titanium dioxide
1.5:4.0 is mixed in grinder in molar ratio, after mixed grinding 2h, obtains mixed-powder blank, by mixed-powder blank high temperature
Sintering, discharging, obtains pretreatment mixed-powder, mixed powder will be pre-processed and first use mass fraction be 15% salt acid elution for 8 times after, then
Be washed with deionized, and by the pretreatment mixed powder after washing be 80 DEG C in temperature under conditions of after dry 5h, obtain mixed powder
End；The ethanol solution 1:60 in mass ratio that mixed-powder and mass fraction are 60% is mixed in beaker, and is added into beaker
The polyallylamine hydrochlorides that 0.3 times of mixed-powder quality are 40 DEG C in temperature, and under conditions of revolving speed is 600r/min, stirring is mixed
After closing 3h, polyallylamine hydrochlorides mixture is obtained, polyallylamine hydrochlorides mixture is mixed with stannic chloride 10:1 in mass ratio
In flask, and 0.2 times of stannic chloride quality of lead chloride is added into flask, is 60 DEG C in temperature, revolving speed is 450r/min's
Under the conditions of, after being stirred 2h, the pH to 10 of material in flask is adjusted with the ammonium hydroxide that mass fraction is 15%, and in room temperature condition
After lower standing 12h, filtering obtains filter cake, under conditions of being 80 DEG C in temperature by filter cake after dry 3h, obtains pre- modified powder；It will be pre-
After calcining 3h in modified powder immigration Muffle furnace, Muffle in-furnace temperature is down to room temperature, discharges, obtains modified powder, it will modified powder
End is mixed in three-necked flask with graphene oxide 2:1 in mass ratio, and 30 times of modified powder quality are added into three-necked flask
Trishydroxymethylaminomethane buffer solution, after ultrasonic disperse 50min, it is mixed to obtain modified powder under conditions of frequency is 55kHz
Object is closed, modified powder mixture is mixed with dopamine 18:2 in mass ratio, is 60 DEG C in temperature, revolving speed is the item of 800r/min
Under part, after being stirred to react for 24 hours, filtering obtains additive blank, dry under conditions of being 80 DEG C in temperature by additive blank
After 80min, additive is obtained；According to parts by weight, it successively weighs: 40 parts of polyurethane acroleic acids, 15 portions of reactive diluents, 10 parts of light
Initiator, 5 parts of levelling agents, 6 parts of wetting agent BYK, 8 parts of dispersing agents, 60 parts of mixed solvents and 25 parts of additives；By polyurethane propylene
Acid is mixed in blender with mixed solvent, and reactive diluent is successively added into blender, photoinitiator, levelling agent, profit
Humectant BYK, dispersing agent and additive are 50 DEG C in temperature, under conditions of revolving speed is 500r/min, after being stirred 2h, must receive
Rice insulating moulding coating.The high temperature sintering is to be warming up to 850 DEG C with the heating rate of 10 DEG C/min, heat preservation sintering 14h.The calcining
Temperature is 750 DEG C.The reactive diluent is reactive diluent HK-66.The photoinitiator is photoinitiator TPO.The stream
Flat agent is silicone oil.The dispersing agent is dispersing agent NNO.The mixed solvent is by ethyl acetate and butyl acetate in mass ratio 3:
1 mixing, obtains mixed solvent.
Trishydroxymethylaminomethane is mixed with water 1:90 in mass ratio, adjusts three hydroxyls with the hydrochloric acid that mass fraction is 10%
The pH to 8.5 of aminomethane and aqueous mixtures, obtains trishydroxymethylaminomethane buffer solution；By potassium carbonate and titanium dioxide
1.5:4.0 is mixed in grinder in molar ratio, after mixed grinding 2h, obtains mixed-powder blank, by mixed-powder blank high temperature
Sintering, discharging, obtains pretreatment mixed-powder, mixed powder will be pre-processed and first use mass fraction be 15% salt acid elution for 8 times after, then
Be washed with deionized, and by the pretreatment mixed powder after washing be 80 DEG C in temperature under conditions of after dry 5h, obtain mixed powder
End；The ethanol solution 1:60 in mass ratio that mixed-powder and mass fraction are 60% is mixed in beaker, and is added into beaker
The polyallylamine hydrochlorides that 0.3 times of mixed-powder quality are 40 DEG C in temperature, and under conditions of revolving speed is 600r/min, stirring is mixed
After closing 3h, polyallylamine hydrochlorides mixture is obtained, polyallylamine hydrochlorides mixture is mixed with stannic chloride 10:1 in mass ratio
In flask, and 0.2 times of stannic chloride quality of lead chloride and 5 times of stannic chloride quality of butyl titanate are added into flask, in
Temperature is 60 DEG C, under conditions of revolving speed is 450r/min, after being stirred 2h, adjusts flask with the ammonium hydroxide that mass fraction is 15%
The pH to 10 of interior material, and after standing 12h under room temperature, filtering obtains filter cake, by filter cake under conditions of temperature is 80 DEG C
After dry 3h, pre- modified powder is obtained；Pre- modified powder is moved into Muffle furnace after calcining 3h, Muffle in-furnace temperature is down to room
Temperature, discharging, obtains modified powder, modified powder is placed in three-necked flask, and modified powder quality 30 is added into three-necked flask
Trishydroxymethylaminomethane buffer solution again obtains modified powder under conditions of frequency is 55kHz after ultrasonic disperse 50min
Mixture mixes modified powder mixture with dopamine 18:2 in mass ratio, is 60 DEG C in temperature, revolving speed is 800r/min's
Under the conditions of, after being stirred to react for 24 hours, filtering obtains additive blank, dry under conditions of being 80 DEG C in temperature by additive blank
After 80min, additive is obtained；According to parts by weight, it successively weighs: 40 parts of polyurethane acroleic acids, 15 portions of reactive diluents, 10 parts of light
Initiator, 5 parts of levelling agents, 6 parts of wetting agent BYK, 8 parts of dispersing agents, 60 parts of mixed solvents and 25 parts of additives；By polyurethane propylene
Acid is mixed in blender with mixed solvent, and reactive diluent is successively added into blender, photoinitiator, levelling agent, profit
Humectant BYK, dispersing agent and additive are 50 DEG C in temperature, under conditions of revolving speed is 500r/min, after being stirred 2h, must receive
Rice insulating moulding coating.The high temperature sintering is to be warming up to 850 DEG C with the heating rate of 10 DEG C/min, heat preservation sintering 14h.The calcining
Temperature is 750 DEG C.The reactive diluent is reactive diluent HK-66.The photoinitiator is photoinitiator TPO.The stream
Flat agent is silicone oil.The dispersing agent is dispersing agent NNO.The mixed solvent is by ethyl acetate and butyl acetate in mass ratio 3:
1 mixing, obtains mixed solvent.
Trishydroxymethylaminomethane is mixed with water 1:90 in mass ratio, adjusts three hydroxyls with the hydrochloric acid that mass fraction is 10%
The pH to 8.5 of aminomethane and aqueous mixtures, obtains trishydroxymethylaminomethane buffer solution；By potassium carbonate and titanium dioxide
1.5:4.0 is mixed in grinder in molar ratio, after mixed grinding 2h, obtains mixed-powder blank, by mixed-powder blank high temperature
Sintering, discharging, obtains pretreatment mixed-powder, mixed powder will be pre-processed and first use mass fraction be 15% salt acid elution for 8 times after, then
Be washed with deionized, and by the pretreatment mixed powder after washing be 80 DEG C in temperature under conditions of after dry 5h, obtain mixed powder
End；The ethanol solution 1:60 in mass ratio that mixed-powder and mass fraction are 60% is mixed in beaker, and is added into beaker
The polyallylamine hydrochlorides that 0.3 times of mixed-powder quality are 40 DEG C in temperature, and under conditions of revolving speed is 600r/min, stirring is mixed
After closing 3h, polyallylamine hydrochlorides mixture is obtained, polyallylamine hydrochlorides mixture is mixed with stannic chloride 10:1 in mass ratio
In flask, and 0.2 times of stannic chloride quality of lead chloride and 5 times of stannic chloride quality of butyl titanate are added into flask, in
Temperature is 60 DEG C, under conditions of revolving speed is 450r/min, after being stirred 2h, adjusts flask with the ammonium hydroxide that mass fraction is 15%
The pH to 10 of interior material, and after standing 12h under room temperature, filtering obtains filter cake, by filter cake under conditions of temperature is 80 DEG C
After dry 3h, pre- modified powder is obtained；Pre- modified powder is moved into Muffle furnace after calcining 3h, Muffle in-furnace temperature is down to room
Temperature, discharging, obtains modified powder, modified powder and graphene oxide 2:1 in mass ratio is mixed in three-necked flask, and to three mouthfuls
30 times of modified powder quality of trishydroxymethylaminomethane buffer solution is added in flask, surpasses under conditions of frequency is 55kHz
After sound disperses 50min, modified powder mixture is obtained, in temperature is 60 DEG C by modified powder mixture, revolving speed is 800r/min
Under the conditions of, after being stirred to react for 24 hours, filtering obtains additive blank, dry under conditions of being 80 DEG C in temperature by additive blank
After 80min, additive is obtained；According to parts by weight, it successively weighs: 40 parts of polyurethane acroleic acids, 15 portions of reactive diluents, 10 parts of light
Initiator, 5 parts of levelling agents, 6 parts of wetting agent BYK, 8 parts of dispersing agents, 60 parts of mixed solvents and 25 parts of additives；By polyurethane propylene
Acid is mixed in blender with mixed solvent, and reactive diluent is successively added into blender, photoinitiator, levelling agent, profit
Humectant BYK, dispersing agent and additive are 50 DEG C in temperature, under conditions of revolving speed is 500r/min, after being stirred 2h, must receive
Rice insulating moulding coating.The high temperature sintering is to be warming up to 850 DEG C with the heating rate of 10 DEG C/min, heat preservation sintering 14h.The calcining
Temperature is 750 DEG C.The reactive diluent is reactive diluent HK-66.The photoinitiator is photoinitiator TPO.The stream
Flat agent is silicone oil.The dispersing agent is dispersing agent NNO.The mixed solvent is by ethyl acetate and butyl acetate in mass ratio 3:
1 mixing, obtains mixed solvent.
Comparative example: the nanometer heat isolation paint of Wuxi material production Co., Ltd production.
Example 1 to the resulting nanometer heat isolation paint of example 5 and comparative example product are subjected to performance detection, specific detection method
It is as follows:
Mercurial thermometer is inserted into from body side, cabinet center is placed in, tests the adiabatic temperature of film, template is placed in case
At the top of body, make heat source just vertical irradiation template.Before opening power supply, reads case body temperature and record.Power on, from
Irradiation initially plays timing and reading, records a case body temperature every 5min, and calculate the intracorporal temperature difference of 1h rear cabinet.According to
GB1768 detects its wear-resisting property.
Specific testing result is as shown in table 1:
1 nanometer heat isolation paint performance test results of table
| Detection project | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example |
| ΔT/℃ | 4.7 | 13.5 | 15.3 | 17.8 | 19.6 | 26.6 |
| Abrasion/mg | 0.021 | 0.467 | 0.483 | 0.598 | 0.627 | 0.804 |
By 1 testing result of table it is found that the nanometer heat isolation paint of technical solution of the present invention preparation has excellent heat-proof quality and resistance to
The characteristics of grinding performance, has broad prospects in the development of macromolecule heat-barrier material technology industry.
Claims (9)
1. a kind of preparation method of nanometer heat isolation paint, which is characterized in that specific preparation step are as follows:
(1) by potassium carbonate, 1.2:4.0~1.5:4.0 is mixed in molar ratio with titanium dioxide, grinding, high temperature sintering, and discharging is washed
It washs, dry, grinding obtains mixed-powder；
(2) mixed-powder is mixed with ethanol solution 1:30~1:60 in mass ratio, and mixed-powder quality 0.2~0.3 is added
Times polyallylamine hydrochlorides, after being stirred, obtain polyallylamine hydrochlorides mixture, by polyallylamine hydrochlorides mixture with
Stannic chloride 8:1~10:1 in mass ratio mixing, and be added 0.1~0.2 times of stannic chloride quality lead chloride and stannic chloride quality 3~
5 times of butyl titanate after being stirred, adjusts pH to 8~10, stands, filters, dry, obtains pre- modified powder；
(3) pre- modified powder is calcined, obtains modified powder, modified powder and graphene oxide 1:1~2:1 in mass ratio are mixed
It closes, and 15~30 times of modified powder quality of trishydroxymethylaminomethane buffer solution is added, after ultrasonic disperse, obtain modified powder
Mixture mixes modified powder mixture with dopamine 15:2~18:2 in mass ratio, after being stirred to react, filters, dry, obtains
Additive；
(4) according to parts by weight, it successively weighs: 30~40 parts of polyurethane acroleic acids, 10~15 portions of reactive diluents, 5~10 parts
Photoinitiator, 3~5 parts of levelling agents, 2~6 parts of wetting agent BYK, 2~8 parts of dispersing agents, 50~60 parts of mixed solvents and 20~25 parts
Additive；Polyurethane acroleic acid is mixed with mixed solvent, and sequentially adds reactive diluent, photoinitiator, levelling agent, wetting
Agent BYK, dispersing agent and additive after being stirred, obtain nanometer heat isolation paint.
2. a kind of preparation method of nanometer heat isolation paint according to claim 1, which is characterized in that step (1) described height
Temperature, which is sintered to, is warming up to 700~850 DEG C with the heating rate of 5~10 DEG C/min, 12~14h of heat preservation sintering.
3. a kind of preparation method of nanometer heat isolation paint according to claim 1, which is characterized in that step (3) is described to forge
Burning temperature is 700~750 DEG C.
4. a kind of preparation method of nanometer heat isolation paint according to claim 1, which is characterized in that step (3) described three
Hydroxymethyl aminomethane buffer solution be trishydroxymethylaminomethane is mixed with water 1:80~1:90 in mass ratio, adjusting pH to
8.0~8.5, obtain trishydroxymethylaminomethane buffer solution.
5. a kind of preparation method of nanometer heat isolation paint according to claim 1, which is characterized in that step (4) described work
Property diluent be reactive diluent HK-66, reactive diluent HELOXY61 or reactive diluent HELOXY62 in any one.
6. a kind of preparation method of nanometer heat isolation paint according to claim 1, which is characterized in that step (4) described light
Initiator is photoinitiator TPO, any one in photoinitiator 184 or photoinitiator 907.
7. a kind of preparation method of nanometer heat isolation paint according to claim 1, which is characterized in that step (4) described stream
Flat agent is any one in silicone oil or dimethyl silicone polymer.
8. a kind of preparation method of nanometer heat isolation paint according to claim 1, which is characterized in that described point of step (4)
Powder is dispersing agent NNO, any one in Dispersant MF or dispersing agent 5040.
9. a kind of preparation method of nanometer heat isolation paint according to claim 1, which is characterized in that step (4) is described mixed
Bonding solvent is to mix ethyl acetate with butyl acetate 1:1~3:1 in mass ratio, obtains mixed solvent.
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Cited By (6)
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| CN109944085A (en) * | 2019-02-25 | 2019-06-28 | 苗霞明 | A kind of washable fabric insulating moulding coating |
| CN110079179A (en) * | 2019-05-30 | 2019-08-02 | 江苏美乔科技有限公司 | Wear-resisting anti-aging water lustering oil of one kind and preparation method thereof |
| CN110156950A (en) * | 2019-05-30 | 2019-08-23 | 杨开芳 | A kind of preparation method of environmental-protection flame-retardant polyurethane foamed material |
| CN110172302A (en) * | 2019-05-30 | 2019-08-27 | 宋昆昆 | A kind of preparation method of water-resistant type inorganic silicic acid sodium adhesive |
| CN110228257A (en) * | 2019-05-30 | 2019-09-13 | 龚建林 | A kind of preparation method of the scratch resistant thermal isolation film of nano ceramics |
| CN110767371A (en) * | 2019-11-04 | 2020-02-07 | 安徽恒晶电缆集团有限公司 | High-temperature computer cable and processing technology thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109944085A (en) * | 2019-02-25 | 2019-06-28 | 苗霞明 | A kind of washable fabric insulating moulding coating |
| CN110079179A (en) * | 2019-05-30 | 2019-08-02 | 江苏美乔科技有限公司 | Wear-resisting anti-aging water lustering oil of one kind and preparation method thereof |
| CN110156950A (en) * | 2019-05-30 | 2019-08-23 | 杨开芳 | A kind of preparation method of environmental-protection flame-retardant polyurethane foamed material |
| CN110172302A (en) * | 2019-05-30 | 2019-08-27 | 宋昆昆 | A kind of preparation method of water-resistant type inorganic silicic acid sodium adhesive |
| CN110228257A (en) * | 2019-05-30 | 2019-09-13 | 龚建林 | A kind of preparation method of the scratch resistant thermal isolation film of nano ceramics |
| CN110767371A (en) * | 2019-11-04 | 2020-02-07 | 安徽恒晶电缆集团有限公司 | High-temperature computer cable and processing technology thereof |
| CN110767371B (en) * | 2019-11-04 | 2022-04-15 | 安徽恒晶电缆集团有限公司 | High-temperature computer cable and processing technology thereof |
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