CN104403558A - Preparation method for solar-energy selectively-adsorbing paint with self cleaning function - Google Patents
Preparation method for solar-energy selectively-adsorbing paint with self cleaning function Download PDFInfo
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- CN104403558A CN104403558A CN201410647260.8A CN201410647260A CN104403558A CN 104403558 A CN104403558 A CN 104403558A CN 201410647260 A CN201410647260 A CN 201410647260A CN 104403558 A CN104403558 A CN 104403558A
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Abstract
The invention discloses a preparation method for solar-energy selectively-adsorbing paint with self cleaning function, and belongs to the technical field of solar energy adsorbing paint. The preparation method comprises the following steps: adding aluminium chloride and manganese nitrate into deionized water, stirring to dissolve the two compositions, dropwise adding a sodium hydroxide solution with stirring, filtering out the precipitate, washing with deionized water, then drying, sintering, and performing ball milling to obtain a matrix powder; preparing a suspension from the matrix powder, using a sodium silicate aqueous solution to adjust the pH value of the suspension to be 8.0-10.0, dropwise adding a sodium silicate aqueous solution and diluted sulfur acid into the suspension in a parallel flow way to perform reaction, filtering, using deionized water to wash and calcining, so as to obtain a nanometer powder with the surface coated with silicon monoxide; and putting into a KOH solution, heating, keeping warm, filtering, baking the solid to dry, putting in an ethanol solution of a silane coupling agent, reacting, and filtering out the solid to obtain a modified powder, and preparing the paint from the modified powder and a resin matrix. the surface of a coating prepared from the paint is good in hydrophobicity and high in adhesive force.
Description
Technical field
The present invention discloses a kind of preparation method with the solar selectively absorbing coating of self-cleaning property, belongs to solar energy absorbing paint technical field.
Background technology
Related statistical shows, and the oil in the whole world approximately can supply the mankind 45 years again, and Sweet natural gas also can only supply 61 years, and coal is slightly long, but also only has about 230 years.The Energy situation of China is severeer, and according to current statistics, CNPC's reserves are only enough exploited 15 years, and Sweet natural gas about can exploit 30 years, and coal 80 years only, meanwhile, due to the rapid growth of economy, domestic energy demand is still increasing at a high speed.Present imported crude oil has accounted for the 40%-50% of aggregate consumption.
According to international new forms of energy development trend, solar thermal utilization has ample scope for one's abilities in substitute fossil fuels generating and terminal utilize.Solar thermal utilization has wide Application Areas, but current most importantly solar energy thermal-power-generating and energy for building (comprising heating, air-conditioning and hot water).In China, technology maturation and formed industry only have solar water heating system.
The utilization of sun power mainly contains light-electricity conversion, light-chemical transformation (photochemical catalysis and hydrogen manufacturing) and photothermal deformation.Solar energy collector is device sun power being directly converted to heat energy, and solar energy collector can be divided into the large class of middle low temperature, middle high temperature heat collector two according to purposes.Middle low-temperature heat collection device technology is widely used on solar water heater and single-action refrigerator air-conditioning, and the main application of middle high temperature heat collector is dual-effect refrigeration agent air-conditioning and solar energy power plant.Solar energy heating technology does not consume mineral fuel, pollution-free, widely applicable, become field of solar energy utilization Main way.
Solar energy collector of good performance is one of key technology and equipment of solar water heater.The solar energy collector of current maturation mainly contains flat plate collector, glass vacuum pipe heat collector, heat pipe vacuum tube hot collector and CPC type heat pipe type heat collector.
Part most crucial in heat collector is solar energy absorbing coating, and numerous experiments proves, the selective absorbing of coating is that photothermal conversion the most effectively designs.This coating absorbs sun power ultraviolet to the most of light wave near infrared range, is then strong reflection at infrared band.The object of such design is the high thermal emissivity avoiding as far as possible bringing because coating absorbs infrared rays, and cause heat-energy losses, especially with the rising of coating duty temperature, this part thermosteresis is more serious.Therefore, design high temperature solar absorber coatings not only will solve the resistant to elevated temperatures problem of material itself, also effectively will suppress thermal emissivity.
CN 103866231A discloses a kind of preparation method of solar selectively absorbing coating.The present invention uses lithographic technique, adopts silica glass as substrate, utilizes lithographic technique, substrate carves width is 500nm-600nm, the degree of depth is the groove of 100-150nm.In the substrate of with groove formula, adopt the method for vacuum plating, the metal/ceramic multilayer film with gradually variable of deposition six layers of different components.Last on metal/ceramic multilayer film with gradually variable, use vacuum-evaporation plating method, deposition one deck Al
2o
3antireflection layer.CN 103866233A discloses the preparation method of high temperature solar absorber coatings in a kind of titaniferous, and it comprises the following steps: S1. selects matrix, matrix is prepared one deck aluminium film as metallic red outer reflective layer; S2. with pure titanium for target, using the mixed gas of argon gas and nitrogen as sputter gas, adopt magnetron sputtering to prepare the first absorption layer in metallic red outer reflective layer; S3. keep the target in step S2 and sputter gas kind constant, reduce sputtering current, reduce nitrogen flow simultaneously, the first absorption layer is prepared the second absorption layer; S4. optics antireflection layer is prepared.But above-mentioned coating all also exists the problem that coating is not high for the sticking power of glass baseplate, do not have self-cleaning function.
Summary of the invention
Technical problem to be solved by this invention is: solar energy absorbing paint is not high for the sticking power of glass baseplate, do not have self-cleaning function, its preparation method is improved, proposes a kind of preparation method with the solar selectively absorbing coating of self-cleaning property.
Technical scheme:
There is a preparation method for the solar selectively absorbing coating of self-cleaning property, comprise the steps:
1st step, by weight, 3 ~ 5 parts of aluminum chloride, manganous nitrate 0.5 ~ 1 part is added in the deionized water of 100 parts, be stirred to dissolving, dripping mass concentration is while stirring the sodium hydroxide solution of 1%, until generate without precipitation, after sedimentation and filtration is gone out, spend Ion Cleaning, then dry 5 ~ 8h at 120 ~ 130 DEG C, more dried powder is sintered in retort furnace, sintered material grinds 1 ~ 3h again on ball mill, obtains base material powder;
2nd step, base material powder is made into the suspension of 50g/L, with the sodium silicate aqueous solution of 1mol/L, the pH value of suspension is adjusted to 8.0 ~ 10.0, in suspension and drip adds the sodium silicate aqueous solution of 1mol/L and the dilute sulphuric acid of 1mol/L, react, after dripping off, let cool, slaking 30min, regulate pH=7.0 with the dilute sulphuric acid of 1mol/L, continue to stir 30min, filter, with deionized water wash, filter cake is placed in retort furnace, and calcining, namely obtains the nano-powder that silicon oxide surface is coated;
3rd step, to be placed in by nano-powder coated for silicon oxide surface and to be added to KOH solution, heating, insulation, after filtration, solids is dried, is placed in the ethanolic soln of the silane coupling agent containing 5wt%, after reaction, leach solids, with ethanol purge, obtain modified powder;
4th step, by modified powder, ethyl acetate 3 ~ 5 parts, silicone resin 2 ~ 4 parts, anti ultraviolet agent 0.01 ~ 0.03 part, 0.01 ~ 0.03 part, oxidation inhibitor, after mixing.
In the 2nd described step, temperature of reaction is 80 ~ 90 DEG C.
In the 2nd described step, the weight of sodium silicate aqueous solution and the weight ratio of base material powder are 50 ~ 80:1.
In the 2nd described step, calcination time 1 ~ 3h.
In the 2nd described step, calcining temperature 600 ~ 800 DEG C.
In the 3rd described step, 7 ~ 10 hours reaction times.
In the 3rd described step, temperature of reaction 40 ~ 50 DEG C.
In the 3rd described step, the concentration 20wt% of KOH solution.
In the 4th described step, anti ultraviolet agent is UV-326, UV-327 or UV-531.
In the 4th described step, oxidation inhibitor is Hinered phenols antioxidant, such as: antioxidant 264, antioxidant 1076.
beneficial effect
The present invention carries out the coated of silicon oxide by the alumina powder jointed surface formed calcining, and the modification of coupling agent is carried out on the surface of silicon oxide, can improve the hydrophobicity of coatingsurface, and can improve the sticking power of coating.
Embodiment
embodiment 1
The preparation method of solar selectively absorbing coating, comprises the steps:
1st step, in the deionized water of 100Kg, add 3Kg aluminum chloride, manganous nitrate 0.5Kg, be stirred to dissolving, dripping mass concentration is while stirring the sodium hydroxide solution of 1%, until generate, after being gone out by sedimentation and filtration without precipitation, spend Ion Cleaning, at 120 DEG C, dry 5h again, more dried powder is sintered in retort furnace, sintering temperature 900 DEG C, sintered material grinds 1h again on ball mill, obtains base material powder;
2nd step, base material powder is made into the suspension of 50g/L, with the sodium silicate aqueous solution of 1mol/L, the pH value of suspension is adjusted to 8.0, in suspension, also drip adds the sodium silicate aqueous solution of 1mol/L and the dilute sulphuric acid of 1mol/L, the weight of sodium silicate aqueous solution and the weight ratio of base material powder are 50:1, react, temperature of reaction is 80 DEG C, after dripping off, let cool, slaking 30min, pH=7.0 is regulated with the dilute sulphuric acid of 1mol/L, continue to stir 30min, filter, with deionized water wash, filter cake is placed in retort furnace, 1h is calcined at 600 DEG C, namely the nano-powder that silicon oxide surface is coated is obtained,
3rd step, nano-powder coated for silicon oxide surface is placed in is added to KOH solution, the concentration 20wt% of KOH solution, be heated to 80 DEG C, insulation 2h, after filtration, solids is dried, is placed in the ethanolic soln of the silane coupling agent KH570 containing 5wt%, 7 hours reaction times, temperature of reaction 40 DEG C, after reaction, leaches solids, with ethanol purge, obtain modified powder;
4th step, by modified powder, ethyl acetate 3Kg, silicone resin 2Kg, anti ultraviolet agent (anti ultraviolet agent UV-326) 0.01Kg, oxidation inhibitor (antioxidant 264) 0.01Kg, after mixing.
embodiment 2
The preparation method of solar selectively absorbing coating, comprises the steps:
1st step, in the deionized water of 100Kg, add 5Kg aluminum chloride, manganous nitrate 1Kg, be stirred to dissolving, dripping mass concentration is while stirring the sodium hydroxide solution of 1%, until generate without precipitation, after being gone out by sedimentation and filtration, spend Ion Cleaning, 8h is dried again at 130 DEG C, sintered in retort furnace by dried powder, sintered material grinds 3h again on ball mill again, obtains base material powder;
2nd step, base material powder is made into the suspension of 50g/L, with the sodium silicate aqueous solution of 1mol/L, the pH value of suspension is adjusted to 10.0, in suspension, also drip adds the sodium silicate aqueous solution of 1mol/L and the dilute sulphuric acid of 1mol/L, the weight of sodium silicate aqueous solution and the weight ratio of base material powder are 80:1, react, temperature of reaction is 90 DEG C, after dripping off, let cool, slaking 30min, pH=7.0 is regulated with the dilute sulphuric acid of 1mol/L, continue to stir 30min, filter, with deionized water wash, filter cake is placed in retort furnace, 3h is calcined at 800 DEG C, namely the nano-powder that silicon oxide surface is coated is obtained,
3rd step, nano-powder coated for silicon oxide surface is placed in is added to KOH solution, the concentration 20wt% of KOH solution, be heated to 80 DEG C, insulation 2h, after filtration, solids is dried, is placed in the ethanolic soln of the silane coupling agent KH570 containing 5wt%, 10 hours reaction times, temperature of reaction 50 DEG C, after reaction, leaches solids, with ethanol purge, obtain modified powder;
4th step, by modified powder, ethyl acetate 5Kg, silicone resin 4Kg, anti ultraviolet agent (anti ultraviolet agent UV-326) 0.03Kg, oxidation inhibitor (antioxidant 264) 0.03Kg, after mixing.
embodiment 3
The preparation method of solar selectively absorbing coating, comprises the steps:
1st step, in the deionized water of 100Kg, add 4Kg aluminum chloride, manganous nitrate 0.8Kg, be stirred to dissolving, dripping mass concentration is while stirring the sodium hydroxide solution of 1%, until generate without precipitation, after being gone out by sedimentation and filtration, spend Ion Cleaning, 6h is dried again at 125 DEG C, sintered in retort furnace by dried powder, sintered material grinds 2h again on ball mill again, obtains base material powder;
2nd step, base material powder is made into the suspension of 50g/L, with the sodium silicate aqueous solution of 1mol/L, the pH value of suspension is adjusted to 9.0, in suspension, also drip adds the sodium silicate aqueous solution of 1mol/L and the dilute sulphuric acid of 1mol/L, the weight of sodium silicate aqueous solution and the weight ratio of base material powder are 70:1, react, temperature of reaction is 85 DEG C, after dripping off, let cool, slaking 30min, pH=7.0 is regulated with the dilute sulphuric acid of 1mol/L, continue to stir 30min, filter, with deionized water wash, filter cake is placed in retort furnace, 2h is calcined at 700 DEG C, namely the nano-powder that silicon oxide surface is coated is obtained,
3rd step, nano-powder coated for silicon oxide surface is placed in is added to KOH solution, the concentration 20wt% of KOH solution, be heated to 80 DEG C, insulation 2h, after filtration, solids is dried, is placed in the ethanolic soln of the silane coupling agent KH570 containing 5wt%, 8 hours reaction times, temperature of reaction 45 DEG C, after reaction, leaches solids, with ethanol purge, obtain modified powder;
4th step, by modified powder, ethyl acetate 4Kg, silicone resin 3Kg, anti ultraviolet agent (anti ultraviolet agent UV-326) 0.02Kg, oxidation inhibitor (antioxidant 264) 0.02Kg, after mixing.
reference examples 1
Be with the difference of embodiment 3: the coated of silicon oxide layer is not carried out to alumina powder jointed surface.
The preparation method of solar selectively absorbing coating, comprises the steps:
1st step, in the deionized water of 100Kg, add 4Kg aluminum chloride, manganous nitrate 0.8Kg, be stirred to dissolving, dripping mass concentration is while stirring the sodium hydroxide solution of 1%, until generate without precipitation, after being gone out by sedimentation and filtration, spend Ion Cleaning, 6h is dried again at 125 DEG C, sintered in retort furnace by dried powder, sintered material grinds 2h again on ball mill again, obtains base material powder;
2nd step, base material powder are placed in the ethanolic soln of the silane coupling agent KH570 containing 5wt%, 8 hours reaction times, and temperature of reaction 45 DEG C, after reaction, leaches solids, with ethanol purge, obtains modified powder;
3rd step, by modified powder, ethyl acetate 4Kg, silicone resin 3Kg, anti ultraviolet agent (anti ultraviolet agent UV-326) 0.02Kg, oxidation inhibitor (antioxidant 264) 0.02Kg, after mixing.
reference examples 2
Be with the difference of embodiment 3: the modification surface of silica powder not being carried out to coupling agent.
The preparation method of solar selectively absorbing coating, comprises the steps:
1st step, in the deionized water of 100Kg, add 4Kg aluminum chloride, manganous nitrate 0.8Kg, be stirred to dissolving, dripping mass concentration is while stirring the sodium hydroxide solution of 1%, until generate without precipitation, after being gone out by sedimentation and filtration, spend Ion Cleaning, 6h is dried again at 125 DEG C, sintered in retort furnace by dried powder, sintered material grinds 2h again on ball mill again, obtains base material powder;
2nd step, base material powder is made into the suspension of 50g/L, with the sodium silicate aqueous solution of 1mol/L, the pH value of suspension is adjusted to 9.0, in suspension, also drip adds the sodium silicate aqueous solution of 1mol/L and the dilute sulphuric acid of 1mol/L, the weight of sodium silicate aqueous solution and the weight ratio of base material powder are 70:1, react, temperature of reaction is 85 DEG C, after dripping off, let cool, slaking 30min, pH=7.0 is regulated with the dilute sulphuric acid of 1mol/L, continue to stir 30min, filter, with deionized water wash, filter cake is placed in retort furnace, 2h is calcined at 700 DEG C, namely the nano-powder that silicon oxide surface is coated is obtained,
3rd step, nano-powder coated for silicon oxide surface is placed in is added to KOH solution, the concentration 20wt% of KOH solution, be heated to 80 DEG C, insulation 2h, after filtration, solids dried, obtains coated powder;
4th step, by coated powder, ethyl acetate 4Kg, silicone resin 3Kg, anti ultraviolet agent (anti ultraviolet agent UV-326) 0.02Kg, oxidation inhibitor (antioxidant 264) 0.02Kg, after mixing.
performance test
Above-mentioned coating adopted crystal pulling method film on K9 glass, the rate of pulling is 10cm ∕ min, and the thickness (the heavy method of film) of film is 0.003 g/cm
2, above-mentioned coating joined in the baking oven of 300 DEG C and roast 1h, be namely absorbed coating.
Cross-hatching adopts GB/T9286-1998 test,
Test data is as follows:
Contrast is carried out as can be seen from embodiment and reference examples 1, by carrying out the coated of silicon oxide layer to the surface of aluminum oxide, sticking power and specific absorption can be improved, carry out contrast by embodiment and reference examples 2 can find out, to the surface of silicon oxide carry out coupling agent coated after, can water droplet contact angle be improved, increase automatically cleaning ability, and can sticking power be improved.
Claims (10)
1. there is a preparation method for the solar selectively absorbing coating of self-cleaning property, it is characterized in that, comprise the steps:
1st step, by weight, 3 ~ 5 parts of aluminum chloride, manganous nitrate 0.5 ~ 1 part is added in the deionized water of 100 parts, be stirred to dissolving, dripping mass concentration is while stirring the sodium hydroxide solution of 1%, until generate without precipitation, after sedimentation and filtration is gone out, spend Ion Cleaning, then dry 5 ~ 8h at 120 ~ 130 DEG C, more dried powder is sintered in retort furnace, sintered material grinds 1 ~ 3h again on ball mill, obtains base material powder;
2nd step, base material powder is made into the suspension of 50g/L, with the sodium silicate aqueous solution of 1mol/L, the pH value of suspension is adjusted to 8.0 ~ 10.0, in suspension and drip adds the sodium silicate aqueous solution of 1mol/L and the dilute sulphuric acid of 1mol/L, react, after dripping off, let cool, slaking 30min, regulate pH=7.0 with the dilute sulphuric acid of 1mol/L, continue to stir 30min, filter, with deionized water wash, filter cake is placed in retort furnace, and calcining, namely obtains the nano-powder that silicon oxide surface is coated;
3rd step, to be placed in by nano-powder coated for silicon oxide surface and to be added to KOH solution, heating, insulation, after filtration, solids is dried, is placed in the ethanolic soln of the silane coupling agent containing 5wt%, after reaction, leach solids, with ethanol purge, obtain modified powder;
4th step, by modified powder, ethyl acetate 3 ~ 5 parts, silicone resin 2 ~ 4 parts, anti ultraviolet agent 0.01 ~ 0.03 part, 0.01 ~ 0.03 part, oxidation inhibitor, after mixing.
2. the preparation method with the solar selectively absorbing coating of self-cleaning property according to claim 1, is characterized in that: in the 2nd described step, temperature of reaction is preferably 80 ~ 90 DEG C.
3. the preparation method with the solar selectively absorbing coating of self-cleaning property according to claim 1, is characterized in that: in the 2nd described step, and the weight of sodium silicate aqueous solution and the weight ratio of base material powder are 50 ~ 80:1.
4. the preparation method with the solar selectively absorbing coating of self-cleaning property according to claim 1, is characterized in that: in the 2nd described step, calcination time 1 ~ 3h.
5. the preparation method with the solar selectively absorbing coating of self-cleaning property according to claim 1, is characterized in that: in the 2nd described step, calcining temperature 600 ~ 800 DEG C.
6. the preparation method with the solar selectively absorbing coating of self-cleaning property according to claim 1, is characterized in that: in the 3rd described step, 7 ~ 10 hours reaction times.
7. the preparation method with the solar selectively absorbing coating of self-cleaning property according to claim 1, is characterized in that: in the 3rd described step, temperature of reaction 40 ~ 50 DEG C.
8. the preparation method with the solar selectively absorbing coating of self-cleaning property according to claim 1, is characterized in that: in the 3rd described step, the concentration 20wt% of KOH solution.
9. the preparation method with the solar selectively absorbing coating of self-cleaning property according to claim 1, is characterized in that: in the 4th described step, anti ultraviolet agent is UV-326, UV-327 or UV-531.
10. the preparation method with the solar selectively absorbing coating of self-cleaning property according to claim 1, is characterized in that: in the 4th described step, oxidation inhibitor is Hinered phenols antioxidant.
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Cited By (4)
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| CN107180885A (en) * | 2017-06-21 | 2017-09-19 | 合肥嘉仕诚能源科技有限公司 | A kind of preparation method of dust protection solar cell |
| CN109135559A (en) * | 2018-08-30 | 2019-01-04 | 江苏京展能源科技有限公司 | A kind of solar energy vacuum tube spectral selection absorbing coating and preparation method thereof |
| CN109439188A (en) * | 2018-11-15 | 2019-03-08 | 北京林业大学 | A kind of super-hydrophobic photo-thermal coating and preparation method thereof |
| CN111187528A (en) * | 2020-03-26 | 2020-05-22 | 蒋益平 | Hydrophobic anti-aging glass film and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107180885A (en) * | 2017-06-21 | 2017-09-19 | 合肥嘉仕诚能源科技有限公司 | A kind of preparation method of dust protection solar cell |
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| CN109439188A (en) * | 2018-11-15 | 2019-03-08 | 北京林业大学 | A kind of super-hydrophobic photo-thermal coating and preparation method thereof |
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| CN111187528A (en) * | 2020-03-26 | 2020-05-22 | 蒋益平 | Hydrophobic anti-aging glass film and preparation method thereof |
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