CN107033752A - The preparation method of Weather-resisting powder coating - Google Patents
The preparation method of Weather-resisting powder coating Download PDFInfo
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- C08K5/00—Use of organic ingredients
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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Abstract
The present invention relates to the preparation method of Weather-resisting powder coating, belong to paint field, design is optimized by the manufacture craft to conventional polyester powdery paints, the weatherability of the Weather-resisting powder coating is improved by way of adding modified graphene powder, the Weather-resisting powder coating is in 480h accelerated light ageing experiment, and its light-protection rate can reach more than 97%.
Description
Technical field
The present invention relates to the preparation method of technical field of coatings, more particularly to Weather-resisting powder coating.
Background technology
The raising of powder coating technology is the synthesis result that coating circle sets about improving equipment with construction technology from raw material, its
Target is to obtain the various aspects of performance coating suitable with liquid coating, including pleasing appearance, relatively low solidification temperature, relatively thin
Coating, good application property, while being also actively working to environmental protection and improving cost performance etc..Powdery paints is general by resin, solidification
Agent, color stuffing, auxiliary agent etc. are constituted, and resin, as the main film forming substance of powdery paints, is to obtain high glaze, high levelling film
It is crucial.
At present, the Weather-resisting powder coating applied to metallic material application is mainly polyester and polyurethane-type powdery paints,
Although with certain weather resistance；The weather resistance of coating is mainly tested by outdoor through climate, such as cold and hot, illumination,
The influence of wind and rain, bacterium etc.；And the thermal conductivity of powdery paints is poor at present, it is usually no more than 0.08W/mK, therefore powder
Coating is when by thermal shock, it is impossible to effectively outwards transmit heat, cause it internal and and metal material combination
Face is easily influenceed by thermal shock, the aging of meeting powder quick coating.Even now conventional is resistance to based on polyester resin
Time type powdery paints, is tested in 480h accelerated light ageing（QUV-B）In, its light-protection rate is no more than 50%.
The content of the invention
The present invention is in view of the deficienciess of the prior art, there is provided the preparation method of Weather-resisting powder coating, particular technique
Scheme is as follows：
The preparation method of Weather-resisting powder coating, by polyester resin, curing agent, levelling agent, pigment, filler, degasser, ultraviolet
Absorbent, modified graphene powder are according to mass ratio（150~160）:（10~20）:（2~3）:（50~60）:（75~85）:（0.5~
0.6）:（0.1~0.12）:（33~36）Ratio be well mixed, then extruded by powder coating extruder, it is tabletting, cooling, broken
Broken, sieving, that is, be prepared into the Weather-resisting powder coating.
As the improvement of above-mentioned technical proposal, the preparation method of the polyester resin is, by the polyalcohol of 30 ~ 40 mass parts
Molten condition is heated in a kettle. with the branching agent of 2 ~ 3 mass parts；The fragrance for sequentially adding 47 ~ 50 mass parts is more
The aliphatic polyol acid and the esterification catalyst of 0.1 ~ 0.12 mass parts of first acid, 5 ~ 6 mass parts, are passed through nitrogen and continue temperature reaction extremely
175 ~ 185 DEG C of esterification waters start to generate and distillated；Then 250 ~ 255 DEG C, 9 ~ 10h of coreaction to 95% esterification are gradually heating to
After water discharge, the acidolysis agent for adding 8 ~ 9 mass parts continues to react 4 ~ 5h, vacuumizes polycondensation to acid number and reaches 30 ~ 35mgKOH/g
Afterwards, stop reaction and obtain the polyester resin.
As the improvement of above-mentioned technical proposal, the preparation method of the modified graphene powder is, by 70 ~ 80 mass parts and matter
Measure the work that fraction is less than 0.5mm for 15% sodium silicate solution, the Graphene powder of 80 ~ 90 mass parts, 120 ~ 130 mass parts particle diameters
Property carclazyte be mixed evenly and spherolite be made in comminutor, then spherolite is sent into vacuum sintering furnace, toward vacuum sintering furnace
In be passed through nitrogen and be warming up to 320 ~ 330 DEG C, crude green body ball is made after 20 ~ 30min of sintering, then crude green body ball is immersed into 400 ~ 500 matter
Measure part and mass fraction is 30 ~ 40min in 18 ~ 23% hydrochloric acid, the temperature of hydrochloric acid is 50 ~ 60 DEG C, pulls crude green body ball out from hydrochloric acid
After be fed again into vacuum sintering furnace, nitrogen is passed through into vacuum sintering furnace and 910 ~ 930 DEG C are warming up to, after 60 ~ 70min of sintering
Smart base ball is made, it is molten that smart base ball is cooled to the sodium hydroxide that 400 ~ 500 mass parts of feeding and mass fraction are 18 ~ 23% after room temperature
40 ~ 50min in liquid, the temperature of sodium hydroxide is 80 ~ 90 DEG C, is pulled out from sodium hydroxide solution after smart base ball, uses deionized water
It is dried naturally after rinsing smart base ball 3 ~ 4 times, finally sends into ball mill and the powder that particle diameter is less than 0.05mm is made, the powder
As described modified graphene powder.
As the improvement of above-mentioned technical proposal, the curing agent is beta-hydroxy alkylamide.
As the improvement of above-mentioned technical proposal, the levelling agent is esters of acrylic acid levelling agent.
As the improvement of above-mentioned technical proposal, the pigment is titanium dioxide.
As the improvement of above-mentioned technical proposal, the filler is barium sulfate.
As the improvement of above-mentioned technical proposal, the degasser is styrax.
As the improvement of above-mentioned technical proposal, the ultra-violet absorber is ESCALOL 567.
Beneficial effects of the present invention：Design is optimized by the manufacture craft to conventional polyester powdery paints, by adding
Plus the mode of modified graphene powder improves the weather resistance of the Weather-resisting powder coating, the Weather-resisting powder coating is 480h's
Accelerated light ageing is tested（QUV-B）In, its light-protection rate can reach more than 97%.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
Embodiment 1
1）, the branching agent of 30Kg polyalcohol and 2Kg is heated to molten condition in a kettle.；Sequentially add 47Kg
Aromatic polycarboxylic acid, 5Kg aliphatic polyol acid and 0.1Kg esterification catalyst, be passed through nitrogen and continue temperature reaction to 175 DEG C of esters
Change water to start to generate and distillate；Then 250 DEG C are gradually heating to, after coreaction 9h to 95% esterification water discharge, adds 8Kg's
Acidolysis agent continues to react 4h, vacuumizes polycondensation to acid number and reaches after 30 ~ 35mgKOH/g, stops reaction and obtains the polyester tree
Fat.
2）, 70Kg and mass fraction be less than for 15% sodium silicate solution, 80Kg Graphene powder, 120Kg particle diameters
0.5mm atlapulgite is mixed evenly and spherolite is made in comminutor, then spherolite is sent into vacuum sintering furnace, toward very
Nitrogen is passed through in empty sintering furnace and is warming up to after 320 DEG C, sintering 20min crude green body ball is made, then crude green body ball is immersed into 400Kg and matter
It is 30min in 18 ~ 23% hydrochloric acid to measure fraction, and the temperature of hydrochloric acid is 50 ~ 60 DEG C, is fed again into after pulling crude green body ball out from hydrochloric acid
In vacuum sintering furnace, nitrogen is passed through into vacuum sintering furnace and smart base ball, smart base ball is made after being warming up to 910 DEG C, sintering 60min
It is cooled to and 40min in the sodium hydroxide solution that 400Kg and mass fraction are 18 ~ 23% is sent into after room temperature, the temperature of sodium hydroxide is
80 ~ 90 DEG C, pulled out from sodium hydroxide solution after smart base ball, with it is dried naturally after the smart base ball of deionized water rinsing 3 ~ 4 times,
The powder that particle diameter is less than 0.05mm finally is made in feeding ball mill, the powder is the modified graphene powder.
3）, by 150Kg polyester resin, 10Kg beta-hydroxy alkylamide, 2Kg esters of acrylic acid levelling agent, 50Kg
Titanium dioxide, 75Kg barium sulfate, 0.5Kg styrax, 0.1Kg ESCALOL 567,33Kg modification stone
Black alkene powder is well mixed, then extruded by powder coating extruder, tabletting, cooling, broken, sieving, that is, be prepared into described weather-proof
Type powdery paints.
Above-mentioned Weather-resisting powder coating is used into high pressure electrostatic painting, the average thickness of coating is 80 μm, in 155 DEG C of bakings
Solidify 15min.The thermal conductivity factor of coating is 0.76W/mK after solidification, and impact resistance is more than 50kgcm, QUV-B's (480h)
Light-protection rate is more than 97.7%.
Embodiment 2
1）, the branching agent of 35Kg polyalcohol and 2.6Kg is heated to molten condition in a kettle.；Sequentially add
49Kg aromatic polycarboxylic acid, 5.6Kg aliphatic polyol acid and 0.11Kg esterification catalyst, are passed through nitrogen and continue temperature reaction extremely
180 DEG C of esterification waters start to generate and distillated；Then it is gradually heating to 255 DEG C, after coreaction 9h to 95% esterification water discharge, plus
The acidolysis agent for entering 8.8Kg continues to react 5h, vacuumizes polycondensation to acid number and reaches after 30 ~ 35mgKOH/g, stops reaction and obtains institute
State polyester resin.
2）, 76Kg and mass fraction be less than for 15% sodium silicate solution, 83Kg Graphene powder, 125Kg particle diameters
0.5mm atlapulgite is mixed evenly and spherolite is made in comminutor, then spherolite is sent into vacuum sintering furnace, toward very
Nitrogen is passed through in empty sintering furnace and is warming up to after 325 DEG C, sintering 30min crude green body ball is made, then crude green body ball is immersed into 470Kg and matter
It is 35min in 18 ~ 23% hydrochloric acid to measure fraction, and the temperature of hydrochloric acid is 50 ~ 60 DEG C, is fed again into after pulling crude green body ball out from hydrochloric acid
In vacuum sintering furnace, nitrogen is passed through into vacuum sintering furnace and smart base ball, smart base ball is made after being warming up to 920 DEG C, sintering 66min
It is cooled to and 50min in the sodium hydroxide solution that 470Kg and mass fraction are 18 ~ 23% is sent into after room temperature, the temperature of sodium hydroxide is
80 ~ 90 DEG C, pulled out from sodium hydroxide solution after smart base ball, with it is dried naturally after the smart base ball of deionized water rinsing 3 ~ 4 times,
The powder that particle diameter is less than 0.05mm finally is made in feeding ball mill, the powder is the modified graphene powder.
3）, by 156Kg polyester resin, 18Kg beta-hydroxy alkylamide, 2.7Kg esters of acrylic acid levelling agent, 56Kg
Titanium dioxide, 80Kg barium sulfate, 0.57Kg styrax, 0.11Kg ESCALOL 567,35Kg change
Property Graphene powder be well mixed, then extruded by powder coating extruder, tabletting, cooling, broken, sieving, that is, be prepared into described
Weather-resisting powder coating.
Above-mentioned Weather-resisting powder coating is used into high pressure electrostatic painting, the average thickness of coating is 90 μm, in 160 DEG C of bakings
Solidify 20min.The thermal conductivity factor of coating is 0.79W/mK after solidification, and impact resistance is more than 50kgcm, QUV-B's (480h)
Light-protection rate is more than 97.1%.
Embodiment 3
1）, the branching agent of 40Kg polyalcohol and 3Kg is heated to molten condition in a kettle.；Sequentially add 50Kg
Aromatic polycarboxylic acid, 6Kg aliphatic polyol acid and 0.12Kg esterification catalyst, be passed through nitrogen continue temperature reaction to 185 DEG C
Esterification water starts to generate and distillated；Then 255 DEG C are gradually heating to, after coreaction 10h to 95% esterification water discharge, 9Kg is added
Acidolysis agent continue react 5h, vacuumize polycondensation to acid number and reach after 30 ~ 35mgKOH/g, stop reaction i.e. obtaining the polyester
Resin.
2）, 80Kg and mass fraction be less than for 15% sodium silicate solution, 90Kg Graphene powder, 130Kg particle diameters
0.5mm atlapulgite is mixed evenly and spherolite is made in comminutor, then spherolite is sent into vacuum sintering furnace, toward very
Nitrogen is passed through in empty sintering furnace and is warming up to after 330 DEG C, sintering 30min crude green body ball is made, then crude green body ball is immersed into 500Kg and matter
It is 40min in 18 ~ 23% hydrochloric acid to measure fraction, and the temperature of hydrochloric acid is 50 ~ 60 DEG C, is fed again into after pulling crude green body ball out from hydrochloric acid
In vacuum sintering furnace, nitrogen is passed through into vacuum sintering furnace and smart base ball, smart base ball is made after being warming up to 930 DEG C, sintering 70min
It is cooled to and 50min in the sodium hydroxide solution that 500Kg and mass fraction are 18 ~ 23% is sent into after room temperature, the temperature of sodium hydroxide is
80 ~ 90 DEG C, pulled out from sodium hydroxide solution after smart base ball, with it is dried naturally after the smart base ball of deionized water rinsing 3 ~ 4 times,
The powder that particle diameter is less than 0.05mm finally is made in feeding ball mill, the powder is the modified graphene powder.
3）, by 160Kg polyester resin, 20Kg beta-hydroxy alkylamide, 3Kg esters of acrylic acid levelling agent, 60Kg
Titanium dioxide, 85Kg barium sulfate, 0.6Kg styrax, 0.12Kg ESCALOL 567,36Kg modification
Graphene powder is well mixed, then extruded by powder coating extruder, tabletting, cooling, broken, sieving, that is, be prepared into described resistance to
Time type powdery paints.
Above-mentioned Weather-resisting powder coating is used into high pressure electrostatic painting, the average thickness of coating is 100 μm, in 165 DEG C of bakings
Roasting solidification 20min.The thermal conductivity factor of coating is 0.71W/mK after solidification, and impact resistance is more than 50kgcm, QUV-B (480h)
Light-protection rate be more than 96.5%.
In the above-described embodiments, in the preparation process of polyester resin, the polyalcohol be neopentyl glycol, ethylene glycol, oneself
One or several kinds of mixtures in glycol；The branching agent is trimethylolpropane, trimethylolethane or pentaerythrite；It is described
Aromatic polycarboxylic acid is the mixture of one or both of terephthalic acid (TPA) and M-phthalic acid；Aliphatic polyol acid for oneself two
One or several kinds of mixtures in acid, decanedioic acid, azelaic acid, fumaric acid and maleic acid；The esterification catalyst is monobutyl
Tin oxide or Dibutyltin oxide；The acidolysis agent is fumaric acid acid anhydride, trimellitic anhydride, pyromellitic dianhydride and maleic anhydride
In one or more of mixtures.
The levelling agent can select esters of acrylic acid levelling agent, 1153 type powder of such as Dongguan City Mo Neng Chemical Co., Ltd.s
Coating levelling agent.Beta-hydroxy alkylamide is curing agent, and titanium dioxide is pigment, and barium sulfate is filler, and styrax is degasser, 2- hydroxyls
Base -4- methoxy benzophenones are ultra-violet absorber, its trade name ultra-violet absorber UV-9.
The effect of modified graphene powder is primarily to improve the heat conductivility of the Weather-resisting powder coating to improve it
Weatherability.In modified graphene powder, Graphene powder is very excellent, but Graphene powder and the associativity of polyester resin are poor；Silicon
Acid sodium solution is beneficial to Graphene powder and atlapulgite combination balling-up, when sodium metasilicate is decomposed to form silica at high temperature, its easily with
Atlapulgite is sintered and combined；Atlapulgite is as base material, and it has loose structure, therefore its adsorptivity is strong, in sodium metasilicate
Under promoting, along with atlapulgite surface area is big, Graphene powder disperse and is filled in atlapulgite completion sinter bonded into thick
Base ball；The effect that nitrogen is passed through in vacuum sintering furnace is to prevent Graphene powder to be oxidized at high temperature；Crude green body ball warp persalt
Soak at high temperature so that some atlapulgites of crude green body ball surface are dissolved, and promote crude green body ball to form the knot of loose porous shape
Structure, then double sintering is into fine and close smart base ball at a high temperature of 910 ~ 930 DEG C, and smart base ball is a kind of polycrystalline material, by crystal,
Vitreum and stomata composition, on smart base ball some be not fully converted into the atlapulgite of crystal then by high temperature sodium hydroxide solution again
Secondary dissolving so that the stomata in smart base ball increases, increased again, it is to change that the smart base ball warp of the structure, which crosses the powder that ball milling is made,
Property Graphene powder；Contain substantial amounts of graphene in modified graphene powder, and the sinter of a large amount of loose structures is contained on its surface
Body, due to passing through secondary high-temperature sintering processes, modified graphene powder surface area is big, and activity is good, its associativity with polyester resin
It can significantly improve, little is influenceed on the impact resistance of coating after solidification.Wherein, crude green body ball is because hydrochloric acid exists using HCl treatment
Easily decomposed under high temperature, it is to avoid influence subsequent high temperature sintering；It is to improve hydrogen-oxygen and smart base ball is using sodium hydroxide solution processing
Change the temperature of sodium solution, improve reaction efficiency, be to prevent hydrochloric acid vapour under 80 ~ 90 DEG C of high temperature the reason for without using hydrochloric acid
Change.Due to the addition of modified graphene powder so that the weatherability of the Weather-resisting powder coating is significantly improved.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
Any modifications, equivalent substitutions and improvements made within refreshing and principle etc., should be included in the scope of the protection.
Claims (9)
1. the preparation method of Weather-resisting powder coating, it is characterised in that：By polyester resin, curing agent, levelling agent, pigment, filler,
Degasser, ultra-violet absorber, modified graphene powder are according to mass ratio（150~160）:（10~20）:（2~3）:（50~60）:
（75~85）:（0.5~0.6）:（0.1~0.12）:（33~36）Ratio be well mixed, then extruded by powder coating extruder,
Tabletting, cooling, broken, sieving, that is, be prepared into the Weather-resisting powder coating.
2. the preparation method of Weather-resisting powder coating according to claim 1, it is characterised in that：The system of the polyester resin
Preparation Method is that the branching agent of the polyalcohol of 30 ~ 40 mass parts and 2 ~ 3 mass parts is heated into molten in a kettle.
State；Sequentially add the aromatic polycarboxylic acid of 47 ~ 50 mass parts, the aliphatic polyol acid of 5 ~ 6 mass parts and 0.1 ~ 0.12 mass parts
Esterification catalyst, is passed through nitrogen continuation temperature reaction and starts to generate and distillate to 175 ~ 185 DEG C of esterification waters；Then it is gradually heating to
250 ~ 255 DEG C, after 9 ~ 10h of coreaction to 95% esterification water discharge, the acidolysis agent for adding 8 ~ 9 mass parts continues to react 4 ~ 5h, takes out
Vacuum polycondensation to acid number is reached after 30 ~ 35mgKOH/g, is stopped reaction and is obtained the polyester resin.
3. the preparation method of Weather-resisting powder coating according to claim 1, it is characterised in that：The modified graphene powder
Preparation method be by 70 ~ 80 mass parts and mass fraction be 15% sodium silicate solution, the Graphene powder of 80 ~ 90 mass parts,
The atlapulgite that 120 ~ 130 mass parts particle diameters are less than 0.5mm is mixed evenly and spherolite is made in comminutor, then by spherolite
Send into vacuum sintering furnace, nitrogen is passed through into vacuum sintering furnace and is made slightly after being warming up to 320 ~ 330 DEG C, 20 ~ 30min of sintering
Base ball, then crude green body ball is immersed into 30 ~ 40min, the temperature of hydrochloric acid in the hydrochloric acid that 400 ~ 500 mass parts and mass fraction are 18 ~ 23%
For 50 ~ 60 DEG C, it is fed again into after pulling crude green body ball out from hydrochloric acid in vacuum sintering furnace, nitrogen is passed through into vacuum sintering furnace and is risen
Smart base ball is made after 60 ~ 70min of sintering to 910 ~ 930 DEG C in temperature, smart base ball be cooled to after room temperature send into 400 ~ 500 mass parts and
Mass fraction is 40 ~ 50min in 18 ~ 23% sodium hydroxide solution, and the temperature of sodium hydroxide is 80 ~ 90 DEG C, molten from sodium hydroxide
Pulled out in liquid after smart base ball, with drying it naturally after the smart base ball of deionized water rinsing 3 ~ 4 times, finally send into ball mill and be made
Particle diameter is less than 0.05mm powder, and the powder is the modified graphene powder.
4. the preparation method of Weather-resisting powder coating according to claim 1, it is characterised in that：The curing agent is β-hydroxyl
Alkylamide.
5. the preparation method of Weather-resisting powder coating according to claim 1, it is characterised in that：The levelling agent is propylene
Esters of gallic acid levelling agent.
6. the preparation method of Weather-resisting powder coating according to claim 1, it is characterised in that：The pigment is titanium white
Powder.
7. the preparation method of Weather-resisting powder coating according to claim 1, it is characterised in that：The filler is sulfuric acid
Barium.
8. the preparation method of Weather-resisting powder coating according to claim 1, it is characterised in that：The degasser is to rest in peace
It is fragrant.
9. the preparation method of Weather-resisting powder coating according to claim 1, it is characterised in that：The ultra-violet absorber
For ESCALOL 567.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710253624.8A CN107033752A (en) | 2017-04-18 | 2017-04-18 | The preparation method of Weather-resisting powder coating |
Applications Claiming Priority (1)
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| CN116554768A (en) * | 2023-05-08 | 2023-08-08 | 上海彩立嵘新材料科技有限公司 | Preparation method of high-decorative colorful powder coating |
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