A kind of heat radiation coating with phase-changing and temperature-regulating function and preparation method thereof
【Technical field】
The invention belongs to technical field of paint preparation, and in particular to a kind of heat radiation coating with phase-changing and temperature-regulating function and its
Preparation method.
【Background technology】
In current phase-change material capsule technical field both at home and abroad, capsule wall material is still set with ureaformaldehyde, melamine formaldehyde (MF) etc.
Based on fat, and the phase-change material of this wall material containing formaldehyde can slowly release formaldehyde in use, not meet environmental requirement.
And from the country achievement in research from the point of view of, in the prevalence of microcapsule phase-change latent heat numerical value it is relatively low the problem of, although can pass through
The methods of from the core with higher enthalpy of phase change and increased core timber-used amount, improves the enthalpy of phase change of capsule, but this is simultaneously
Add production cost.Although phase transformation capsule prepared by situ aggregation method is with good suction exothermicity, capsule outer walls
Heat resistance is poor, and the leakage of core is easily caused under conditions of heated, reduces the performance and used life of capsule.
Existing a variety of heat radiation coatings in the market, painting brushing effects are uneven, and difference in selling prices is also relatively large.Foreign countries dissipate
Although hot coating works well, price is in thousands of members of per kilogram or so, although domestic heat radiation coating relative low price,
Radiating effect is bad.In addition, the filler of most of heat radiation coatings is only with thermal conductive ceramic filler boron nitride, silicon nitride and hollow glass
Glass microballon is compounded to obtain, and heat conductivility is obviously improved but radiation efficiency is relatively low, and the improvement on heat dispersion influences little.
【The content of the invention】
It is an object of the invention to provide a kind of heat radiation coating with phase-changing and temperature-regulating function and preparation method thereof, this radiating
Coating is made up of phase-change microcapsule, thermal-radiating material and epoxy resin, wherein the latent heat of phase change of phase-change microcapsule is big, high temperature resistant and
Environment friendly and pollution-free, carborundum, beryllium oxide and aluminium nitride etc. have the advantages of thermal radiation capability strong and good heat conductivity, and both combine
The radiating effect of epoxy resin-matrix heat radiation coating can be significantly improved, the internal temperature for being painted equipment is greatly lowered.
To reach above-mentioned purpose, present invention employs following technical scheme:
A kind of heat radiation coating with phase-changing and temperature-regulating function, including phase-change microcapsule, high-heating radiation material, epoxy resin and
Curing agent;Wherein, the mass fraction of phase-change microcapsule is the 1%~10% of epoxy resin quality, the quality point of thermal-radiating material
Number is the 3%~6% of epoxy resin quality, and the mass fraction of curing agent is the 35%~45% of epoxy resin quality;
The wall material of described phase-change microcapsule is to be passed through by styrene and divinylbenzene under oil-soluble initiator effect
Raolical polymerizable obtains, and core is phase-change material.
Described phase-change microcapsule is prepared by following raw material and parts by weight:
(a) by weight, by the wall material monomer styrene of 150~300 parts of different ratios and divinylbenzene and 70
~600 parts of cores are added in reactor, and the solid being warming up in system is incubated standby after being completely dissolved, obtain mixture;Wall
The mass ratio of material monomer styrene and divinylbenzene is (2~3):1;
(b) will pour into obtained mixture, to system after 10~200 parts of dispersants are dissolved in 1000 parts of water altogether
Carry out emulsification treatment;
(c) after emulsion process terminates, 1~15 part of oil-soluble initiator is added in the mixture, adjusts agitator speed
To 150~1300r/min, for the lower reaction of nitrogen purging to complete, rear blowing goes out kettle, filtering, washing, dries, you can obtain phase transformation
Microcapsules.
Described core is that one or more of compoundings in paraffin, stearic acid and positive long chain alkane obtain.
Described high-heating radiation material is carborundum, beryllium oxide or aluminium nitride, preferably carborundum.
The particle diameter of described phase-change microcapsule is 500 nanometers to 200 microns.
A kind of preparation method of the heat radiation coating with phase-changing and temperature-regulating function, comprises the following steps,
(a) by weight, by the wall material monomer styrene of 150~300 parts of different ratios and divinylbenzene and 70
~600 parts of cores are added in reactor, and the solid being warming up in system is incubated standby after being completely dissolved, obtain mixture;Wall
The mass ratio of material monomer styrene and divinylbenzene is (2~3):1;
(b) will pour into obtained mixture, to system after 10~200 parts of dispersants are dissolved in 1000 parts of water altogether
Carry out emulsification treatment;
(c) after emulsion process terminates, 1~15 part of oil-soluble initiator is added in the mixture, adjusts agitator speed
To 150~1300r/min, for the lower reaction of nitrogen purging to complete, rear blowing goes out kettle, filtering, washing, dries, you can obtain phase transformation
Microcapsules;
(d) phase-change microcapsule and high-heating radiation material are added in epoxy resin, obtained after decentralized processing with phase transformation
The heat radiation coating of temperature adjustment function;Wherein, the mass fraction of phase-change microcapsule is the 1%~10% of epoxy resin quality, heat radiation
The mass fraction of material is the 3%~6% of epoxy resin quality;
(e) heat radiation coating using when need to add and account for the curing agent of epoxy resin quality 35%~45%.
As a further improvement on the present invention, in step (b), the temperature of emulsification treatment is 40~90 DEG C, rotating speed is 100~
2500r/min, time are 10~80 minutes.
As a further improvement on the present invention, in step (c), the nitrogen purging lower reaction time is 2~10h.
As a further improvement on the present invention, described core be paraffin, stearic acid and one kind in positive long chain alkane or
Several compoundings obtain.
As a further improvement on the present invention, described high-heating radiation material is carborundum, beryllium oxide or aluminium nitride, preferably
For carborundum.
Relative to prior art, beneficial effects of the present invention are embodied in:
Phase-change microcapsule prepared by the present invention introduces second comonomer divinyl using polystyrene as main shell structurre
Benzene participates in the formation of shell, enhances the intensity and heat resistance of capsule shell, effectively prevent with high heat energy absorbing and releasing power phase transformation
The leakage phenomenon of core.The present invention devises the formula of heat radiation coating simultaneously, effectively combines the heat-storage thermoregulation work(of phase-change microcapsule
Can be with the high-heating radiation ability of thermal-radiating material so that heat radiation coating can be notable after being brushed to electrical equipment shell and solidifying
Reduce device interior temperature.(1) phase-change microcapsule properties of product are excellent, and its enthalpy of phase change has exceeded current domestic like product most
Big value, the heat absorption capacity of phase-change microcapsule is 124J/g.And can be according to the different flexible feed changes of capsule temperature in use
Proportioning, obtain the product being applicable under varying environment;(2) the phase-change microcapsule phase transformation temperature pointses that use of the present invention are at 80 DEG C or so,
After being brushed to electric equipment metal shell surface, when device temperature is more than 80 DEG C, the paraffin in phase-change microcapsule is by Solid State Transformation
For liquid, and along with substantial amounts of heat is absorbed, so as to reduce the temperature of device interior, while use high-heating radiation material such as carbon
SiClx, beryllium oxide and aluminium nitride etc. as with high thermal conductivity and thermal radiation capability radiating filler, can rapidly by by
Heat inside painting device is transmitted to coating surface, and is dispersed into by the form of infra-red radiation in surrounding air, reaches good
Good cooling-down effect.
This product has advantages below compared with the achievement in research and in the market commercial product reported at present:(1) originally
Present invention is simple, and cost is cheap, and being dosed into the step of product blowing one from raw material completes, and avoids in multi-step preparation and deposits
Yield reduction factor, yield is up to 92% or so.(2) domestic and international commercialized phase-change microcapsule is mainly using amino
Resinae cyst wall, contain formaldehyde in its synthesis material, can slowly discharge in use, cause environmental pollution.And
The phase-change microcapsule synthetic raw material of the present invention is environment-friendly raw material for styrene and divinylbenzene, the product peace prepared
Completely without pollution, while introduce in reaction system the second constituent monomers and functionalization and follow-up is carried out to the shell of phase-change microcapsule
Process of Surface Modification, uniform mixing and the interface compatibility of raw material are efficiently solved the problems, such as, enables to microcapsules directly to apply
In the preparation of epoxy resin-matrix heat radiation coating.
【Brief description of the drawings】
The DSC curve of Fig. 1 phase-change microcapsules;
The brushing Contrast on effect of Fig. 2 heat radiation coatings (to be not coated with coating, the right is to scribble coating on the left side).
【Embodiment】
A kind of heat radiation coating with phase-changing and temperature-regulating function of the present invention, synthesis material are paraffin, styrene, divinyl
Benzene, dispersant, surfactant, oil-soluble initiator, high-heating radiation material such as carborundum, beryllium oxide and aluminium nitride etc., epoxy
Resin and curing agent.
Wherein, the core of phase-change microcapsule is by one or more of phase-change materials such as paraffin, stearic acid in heat radiation coating
Compound what is obtained according to practical application request with positive long chain alkane etc..The wall material of phase-change microcapsule is mainly by benzene in heat radiation coating
What the polystyrene that vinyl monomer is obtained under oil-soluble initiator effect by Raolical polymerizable was formed.In heat radiation coating
The wall material of phase-change microcapsule also passes through radical polymerization by the divinylbenzene containing crosslinking function under oil-soluble initiator effect
The polymer that reaction obtains is closed to form.
The particle diameter of phase-change microcapsule is between 500 nanometers to 200 microns in heat radiation coating, and by adjusting preparation technology
Parameter can obtain the microcapsules with different-grain diameter.There is height using carborundum, beryllium oxide and aluminium nitride etc. in heat radiation coating
The filler of thermal radiation capability is as heat sinking function component, preferably carborundum.
A kind of production technology of the heat radiation coating with phase-changing and temperature-regulating function, comprises the following steps,
(a) by the wall material monomer styrene and divinylbenzene and 70~600 parts of paraffin of 150~300 parts of different ratios
It is added in reactor, the solid being warming up in system is incubated standby after being completely dissolved.
(b) mixture that step (a) obtains will be poured into after 10~200 parts of dispersants are dissolved in 1000g water altogether, risen
Temperature starts agitator, regulation rotating speed to about 100~2500r/min, 10~80 points of emulsification treatment is carried out to system to 40~90 DEG C
Clock.
(c) after emulsion process terminates, 1~15 part of oil-soluble initiator is added in the mixture to trigger the polymerization of system
Reaction, regulation agitator speed is to 150~1300r/min, and blowing goes out kettle and can obtain phase after 2~10h of the lower reaction of nitrogen purging
Become microcapsules.
(d) phase-change microcapsule and high-heating radiation material such as carborundum, beryllium oxide and aluminium nitride etc. are added to epoxy resin
In, obtain the heat radiation coating with phase-changing and temperature-regulating function after scattered 0.5~4 hour.Wherein, the mass fraction of phase-change microcapsule is
The 1%~10% of epoxy resin quality, the mass fraction of thermal-radiating material are the 3%~6% of epoxy resin quality.
(e) it need to add after room temperature curing agent uniformly mixes and brush during heat radiation coating use, surface drying after solidifying 24 hours, 72 is small
When after do solid work.
The present invention is elaborated with reference to specific embodiment.
Embodiment 1
The dispersant of 80g proportional quantities altogether is dissolved in 800g water, adds 200g wall materials monomer styrene and divinyl
Base benzene (mass ratio 2:1) and 200g paraffin, after the solid being warming up in system is completely dissolved, regulation agitator speed is to body
System carries out emulsification treatment 3h.After emulsion process terminates, the oil-soluble initiator of amount of calculation is added in the mixture to trigger system
Polymerisation, blowing goes out kettle and can obtain phase-change microcapsule after the lower reaction 10h of nitrogen purging.By 8g phase-change microcapsules and 5g carbon
SiClx is added in 100g epoxy resin, and stirring adds after 40g room temperature curing agent uniformly mixes to be made after 2 hours, and there is heat accumulation to adjust
The heat radiation coating of temperature function.Surface drying after room temperature is placed 24 hours after brushing, does solid work after 72 hours.
The means of differential scanning calorimetry endothermic curve of phase-change microcapsule is as shown in figure 1, as can be seen from the figure phase-change microcapsule
Heat absorption capacity is 124J/g.
To verify the effect of coating, identical two aluminium pots of heated condition contrast test is subjected to, such as Fig. 2 institutes
Show.Wherein left side aluminium pot is the blank sample for being not coated with coating, and the right aluminium pot is the sample for scribbling coating.Can from infrared imaging figure
To find out, it is higher to scribble the aluminium pot surface heat radiation energy of coating, illustrates that heat distributes faster in coating surface.
Embodiment 2
By 150g wall materials monomer styrene and divinylbenzene (mass ratio 2:And 70g stearic acid and just long alkane 1)
Hydrocarbon is added in reactor, and the solid being warming up in system is incubated standby after being completely dissolved.10g dispersants it will be dissolved in altogether
After in 1000g water, the mixture that step (a) obtains is poured into, is warming up to 40 DEG C, start agitator, regulation rotating speed to about 100r/
Min, emulsification treatment is carried out 10 minutes to system.After emulsion process terminates, in the mixture add 1g oil-soluble initiator with
The polymerisation of initiation system, to 150r/min, after the lower reaction 2h of nitrogen purging, blowing goes out kettle to regulation agitator speed to obtain
To phase-change microcapsule.Phase-change microcapsule and high-heating radiation material such as aluminium nitride are added in epoxy resin, after disperseing 0.5 hour
Obtain the heat radiation coating with phase-changing and temperature-regulating function.Wherein, the mass fraction of phase-change microcapsule is the 1% of epoxy resin quality,
The mass fraction of thermal-radiating material is the 3% of epoxy resin quality.Room temperature curing agent need to be added during heat radiation coating use uniformly to mix
Brush, surface drying after solidifying 24 hours, done solid work after 72 hours after conjunction.
Embodiment 3
By 300g wall materials monomer styrene and divinylbenzene (mass ratio 3:1) and 600g stearic acid is added to reaction
In kettle, the solid that is warming up in system is incubated standby after being completely dissolved.After 200g dispersants are dissolved in 1000g water altogether,
The mixture that step (a) obtains is poured into, is warming up to 90 DEG C, starts agitator, regulation rotating speed enters to about 2500r/min to system
Row emulsification treatment 80 minutes.After emulsion process terminates, 15g oil-soluble initiator is added in the mixture to trigger the poly- of system
Reaction is closed, regulation agitator speed is to 1300r/min, and blowing goes out kettle and can obtain the micro- glue of phase transformation after the lower reaction 10h of nitrogen purging
Capsule.Phase-change microcapsule and high-heating radiation material such as beryllium oxide are added in epoxy resin, obtained after scattered 4 hours with phase transformation
The heat radiation coating of temperature adjustment function.Wherein, the mass fraction of phase-change microcapsule is the 10% of epoxy resin quality, thermal-radiating material
Mass fraction is the 6% of epoxy resin quality.It need to add after room temperature curing agent uniformly mixes and brush during heat radiation coating use, solidify
Surface drying after 24 hours, done solid work after 72 hours.
Embodiment 4
By 200g wall materials monomer styrene and divinylbenzene (mass ratio 2:1) and the positive long chain alkanes of 300g are added to
In reactor, the solid that is warming up in system is incubated standby after being completely dissolved.100g dispersants it will be dissolved in altogether in 1000g water
Afterwards, the mixture that step (a) obtains is poured into, is warming up to 80 DEG C, starts agitator, regulation rotating speed is to about 1500r/min, to system
Carry out emulsification treatment 50 minutes.After emulsion process terminates, 5g oil-soluble initiator is added in the mixture to trigger system
Polymerisation, regulation agitator speed is to 1000r/min, and blowing goes out kettle and can obtain the micro- glue of phase transformation after the lower reaction 6h of nitrogen purging
Capsule.Phase-change microcapsule and high-heating radiation material such as beryllium oxide are added in epoxy resin, obtained after scattered 2 hours with phase transformation
The heat radiation coating of temperature adjustment function.Wherein, the mass fraction of phase-change microcapsule is the 16% of epoxy resin quality, thermal-radiating material
Mass fraction is the 4% of epoxy resin quality.It need to add after room temperature curing agent uniformly mixes and brush during heat radiation coating use, solidify
Surface drying after 24 hours, done solid work after 72 hours.
Embodiment 5
By 250 parts of wall material monomer styrene and divinylbenzene (mass ratio 2.5:1) and 500g paraffin is added to
In reactor, the solid that is warming up in system is incubated standby after being completely dissolved.150g dispersants it will be dissolved in altogether in 1000g water
Afterwards, the mixture that step (a) obtains is poured into, is warming up to 70 DEG C, starts agitator, regulation rotating speed is to about 1000r/min, to system
Carry out emulsification treatment 70 minutes.After emulsion process terminates, 12g oil-soluble initiator is added in the mixture to trigger system
Polymerisation, regulation agitator speed is to 1100r/min, and blowing goes out kettle and can obtain the micro- glue of phase transformation after the lower reaction 4h of nitrogen purging
Capsule.Phase-change microcapsule and high-heating radiation material such as carborundum are added in epoxy resin, obtained after scattered 2 hours with phase transformation
The heat radiation coating of temperature adjustment function.Wherein, the mass fraction of phase-change microcapsule is the 6% of epoxy resin quality, thermal-radiating material
Mass fraction is the 3% of epoxy resin quality.It need to add after room temperature curing agent uniformly mixes and brush during heat radiation coating use, solidify
Surface drying after 24 hours, done solid work after 72 hours.
The several embodiments of the present invention are the foregoing is only, are not all of or unique embodiment, art technology
Personnel are the power of the present invention by reading description of the invention any equivalent conversion for taking technical solution of the present invention
Profit requires to be covered.