CN107629571A - A kind of preparation method of self-cleaning fluorocarbon paint - Google Patents
A kind of preparation method of self-cleaning fluorocarbon paint Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of self-cleaning fluorocarbon paint, belong to technical field of paint preparation.The silicon fluoride hydrolyzed in the present invention is mixed with titanium dioxide and disperseed at a high speed,Obtain the titania nanoparticles of surface modification,Then varnish mixes with CNT dispersion liquid,Micro- solidification obtains self-cleaning fluorocarbon paint,Silicon fluoride increases the combination of titanium dioxide granule and fluorocarbon resin,Silicon fluoride molecule hydrolyzes in acid condition,Due to hydrogen bond action,Silicon fluoride Molecular Adsorption after hydrolysis is on titania nanoparticles surface,Carbochain in silicon fluoride molecule by fluorine original physical barrier effect due to being protected,Other atoms are not easy to invade,So silicon fluoride has good chemical stability and low surface free energy,Silicon fluoride surface coating layer reduces effect of the Ti O2 nano particles to the Van der Waals force and hydrogen bond of water,The greatly contact angle of increase coating surface,So as to show super-hydrophobicity,Stain resistant can be significantly improved,Have a extensive future.
Description
Technical field
The invention discloses a kind of preparation method of self-cleaning fluorocarbon paint, belong to technical field of paint preparation.
Background technology
Fluorocarbon coating refers to the coating using fluororesin as main film forming substance；Also known as F-C paint, fluoro coatings, fluorine resin coating
Deng.Among various coating, for fluorine resin coating because the fluorine element electronegativity of introducing is big, carbon-fluorine bond can be strong, has especially advantageous
Properties.Weatherability, heat resistance, lower temperature resistance, chemical proofing, and with unique non-stick and low friction
Property.By the fast development of decades, fluoro coatings are in building, chemical industry, electric appliance and electronic industry, mechanical industry, Aero-Space
Industry, the every field of household supplies are used widely.As after acrylic coating, polyurethane coating, organosilicon coating etc.
After high-performance coating, combination property highest coating brand.At present, the more extensive fluorine resin coating of application mainly has
The three major types type such as PTFE, PVDF, PEVE.
Steel field：Fluorocarbon coating is appeared on color steel earliest in the application of steel field, installed in factory building and warehouse
Top, it is easy for installation because it is durable in use, it is lucuriant in design, come quickly in Global prevalence.Global steel building and production
Giant-the Butler in product field, the color steel business and the steel construction business that builds a bridge that she is accepted nearly all are applied using fluorine carbon
Expect coating.Pudong International Airport in Shanghai roof just uses the color steel of fluorocarbon coating application.Fluorocarbon coating answering on concrete
With being mainly reflected on external wall.Wherein fluorocarbon coating excellent combination property and the ratio of performance to price, make it super-high buildings,
Landmark building, key project etc. have unmatched competitive advantage, with the development and application of aqueous fluorocarbon coating,
It is sprayable, can also mix painting, again substantially reduces its cost in terms of construction.This is also the major growth in fluorocarbon coating market
Point.
The application of fluorocarbon coating abroad is fairly common, this with their economic strength, coating popularity rate, use warp
Test, the factor such as quality ideology it is relevant.The application surface and sales volume of domestic fluorocarbon coating are also in a relatively low level.People
To its performance and using understanding not enough.With the progress of fluorocarbon coating technology and perfect, the fluorine carbon of construction and application technique
The excellent ratio of performance to price of coating will make it increasingly have competitiveness in every field.But there is also some drawbacks, such as fluorine carbon
Paint surface easily tarnishes, and takes time and effort.Therefore, inventing a kind of self-cleaning fluorocarbon paint has actively meaning to technical field of paint preparation
Justice.
The content of the invention
Present invention mainly solves technical problem, the defects of easily being tarnished for F-C paint surface, there is provided a kind of from clear
The preparation method of clean F-C paint.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
A kind of preparation method of self-cleaning fluorocarbon paint, it is characterised in that specifically preparation process is：
（1）200~220mL absolute ethyl alcohols are mixed with 100~120mL perfluoro capryl triethoxysilane aqueous solution, obtain silicon
Oxygen alkane solution, siloxane solution pH is adjusted with acetic acid, siloxane solution is poured into beaker, mixed with magnetic stirrer,
The silicon fluoride solution hydrolyzed；
（2）Preparing titanium dioxide alcohol mixeding liquid, titanium dioxide alcohol mixeding liquid is mixed with the silicon fluoride solution hydrolyzed, is placed in
Beaker, after being mixed with magnetic stirrer, it is placed in supercentrifuge and centrifuges, removes upper liquid, isolated lower floor
Precipitation, lower sediment is put into vacuum drying chamber, is dried, and obtains the titania nanoparticles of surface modification；
（3）Toluene, isophorone, repefral are mixed to get solvent, counted in parts by weight, by 20~22 parts
The titania nanoparticles that PVDF fluorocarbon resins, 45~50 parts of solvents, 15~20 parts of titanium dioxides and 20~25 parts of surfaces are modified
Mixing, is placed in the stirred tank with cooling device, is dispersed with stirring to obtain pre-dispersed raw material；
（4）Pre-dispersed raw material is added in grinder and is ground, temperature is controlled in process of lapping at 20~30 DEG C, is obtained clear
Paint, is counted in parts by weight, and 20~25 parts of multi-walled carbon nanotubes are added in 100~120 parts of ethyl acetate, obtain mixed liquor, will
Mixed liquor, which is placed in high speed dispersor high speed, to be disperseed, and obtains CNT dispersion liquid；
（5）Count in parts by weight, 70~80 parts of varnish are mixed with 100~110 parts of CNT dispersion liquids, are placed in stirred tank
After stirring, speed of agitator is reduced, 20~25 parts of hexamethylene diisocyanates are added into stirred tank, obtain self-cleaning fluorocarbon
Paint.
Step（1）The mass fraction of the described perfluoro capryl triethoxysilane aqueous solution is 2%, the mass fraction of acetic acid
For 20%, it is 3.0~3.3 to adjust siloxane solution pH with acetic acid, and agitator speed of agitator be 300~320r/min, and stirring mixes
The conjunction time is 22~24 h.
Step（2）The mass concentration of described titanium dioxide alcohol mixeding liquid is 4 mg/mL, titanium dioxide alcohol mixeding liquid
The volume ratio mixed with the silicon fluoride solution of hydrolysis is 4: 1, and magnetic stirrer rotating speed is 400~450r/min, and stirring is mixed
The conjunction time is 7~8 h, and supercentrifuge rotating speed is 4200~4500r/min, and the centrifugation time is 10~12min, and vacuum is done
Dry case design temperature is 80~85 DEG C, and drying time is 12~14 h.
Step（3）Described toluene, isophorone, the volume ratio of repefral mixing are the ︰ 3 of 2 ︰ 1, stirred tank
Rotating speed be 1000~1300r/min, it is 30~35min to be dispersed with stirring the time.
Step（4）Raw material particle size is 25~30 μm after described grinding, and high speed dispersor rotating speed is 7000~7500r/
Min, high speed jitter time are 18~20min.
Step（5）Described speed of agitator is 600~800r/min, and mixing time is 20~25min, reduces speed of agitator
For 300~400r/min.
The beneficial effects of the invention are as follows：
（1）The silicon fluoride hydrolyzed in the present invention is mixed with titanium dioxide and disperseed at a high speed, and the titanium dioxide for obtaining surface modification is received
Rice grain, the titania nanoparticles that PVDF fluorocarbon resins and surface are modified are dispersed through, grinds varnish is made, then varnish and
The mixing of CNT dispersion liquid, micro- solidification obtain self-cleaning fluorocarbon paint, contain substantial amounts of C-F keys, fluorine in main material fluorocarbon resin
Atom has the feature that atomic radius is small, electronegativity is big, polarizability is small, and C-F keys have strong sucking action to ambient electron, separately
Outer silicon fluoride increases the combination of titanium dioxide granule and fluorocarbon resin so that and fluorine compounds have low-surface-energy, so as to
Improve the stain resistant performance of F-C paint；
（2）Silicon fluoride molecule hydrolyzes in acid condition in the present invention, due to hydrogen bond action, the silicon fluoride Molecular Adsorption after hydrolysis
On titania nanoparticles surface, the intermolecular adjacent hydroxyl groups of silicon fluoride interconnect after sloughing hydrone, are received in titanium dioxide
Rice grain surface forms continuous silicon fluoride molecular layer, by the effect of chemisorbed, in titania nanoparticles surface shape
Into one layer of silicon fluoride molecule clad, due to the electrostatic repulsion and space steric effect between nano particle, dioxy can be made
Change titanium nano particle has a good dispersiveness in organic matrix, and the fluorine atom electronegativity in silicon fluoride molecule is larger, with it
The singly-bound bond energy that his element is formed is bigger with bond energy that other elements are formed than carbon atom, and the carbochain in silicon fluoride molecule is due to by fluorine
The protection of former physical barrier effect, other atoms are not easy to invade, so silicon fluoride has good chemical stability and low surface
Free energy, silicon fluoride surface coating layer reduce effect of the titania nanoparticles to the Van der Waals force and hydrogen bond of water, greatly
The contact angle of coating surface is increased, so as to show super-hydrophobicity, stain resistant can be significantly improved, had a extensive future.
Embodiment
By the perfluoro capryl triethoxysilane water that 200~220mL absolute ethyl alcohols and 100~120mL mass fractions are 2%
Solution is mixed, and obtains siloxane solution, and siloxane solution pH to 3.0~3.3 is adjusted with the acetic acid that mass fraction is 60%, will
Siloxane solution is poured into beaker, is stirred 22~24 h with 300~320r/min rotating speed with magnetic stirring apparatus, is obtained water
The silicon fluoride solution of solution；The titanium dioxide alcohol mixeding liquid that mass concentration is 4 mg/mL is prepared, by titanium dioxide alcohol mixeding liquid
Mixed with the silicon fluoride solution of hydrolysis using volume ratio as 4: 1, be placed in beaker, with magnetic stirring apparatus with 400~450r/min's
After rotating speed is stirred 7~8 h, is placed in supercentrifuge and centrifuges 10 with 4200~4500r/min rotating speed~
12min, upper liquid is removed, isolated lower sediment, lower sediment is put into the vacuum that design temperature is 80~85 DEG C and done
In dry case, 12~14 h are dried, obtain the titania nanoparticles of surface modification；By toluene, isophorone, phthalic acid
The ︰ 3 of 2 ︰ 1 are mixed to get solvent to dimethyl ester by volume, count in parts by weight, by 20~22 parts of PVDF fluorocarbon resins, 45~50 parts
The titania nanoparticles mixing that solvent, 15~20 parts of titanium dioxides and 20~25 parts of surfaces are modified, is placed in cooling device
Stirred tank in, with 1000~1300r/min rotating speed, be dispersed with stirring 30~35min, obtain pre-dispersed raw material；Will be pre-dispersed
Raw material is added in grinder and is ground, and is ground to raw material particle size as 25~30 μm, and temperature is controlled in process of lapping 20~30
DEG C, varnish is obtained, is counted in parts by weight, 20~25 parts of multi-walled carbon nanotubes are added in 100~120 parts of ethyl acetate, obtained
Mixed liquor, mixed liquor is placed in high speed dispersor, 18~20min is disperseed at a high speed with 7000~7500r/min rotating speed, obtained
CNT dispersion liquid；Count in parts by weight, 70~80 parts of varnish are mixed with 100~110 parts of CNT dispersion liquids, are placed in
After stirring 20~25min in stirred tank with 600~800r/min rotating speed, reduction speed of agitator is 300~400r/min, to stirring
20~25 parts of hexamethylene diisocyanates of addition in kettle are mixed, obtain self-cleaning fluorocarbon paint.
Example 1
200mL absolute ethyl alcohols are mixed with the perfluoro capryl triethoxysilane aqueous solution that 100mL mass fractions are 2%, obtain silicon
Oxygen alkane solution, siloxane solution pH to 3.0 is adjusted with the acetic acid that mass fraction is 60%, siloxane solution is poured into beaker
In, 22h is stirred with 300r/min rotating speed with magnetic stirring apparatus, the silicon fluoride solution hydrolyzed；Prepare mass concentration
For 4 mg/mL titanium dioxide alcohol mixeding liquid, by the silicon fluoride solution of titanium dioxide alcohol mixeding liquid and hydrolysis with volume ratio
For 4: 1 mixing, beaker is placed in, after being stirred 7h with magnetic stirring apparatus with 400r/min rotating speed, is placed in supercentrifuge
In 10min centrifuged with 4200r/min rotating speed, remove upper liquid, isolated lower sediment, lower sediment be put into and set
Constant temperature degree is in 80 DEG C of vacuum drying chamber, dries 12 h, obtains the titania nanoparticles of surface modification；By toluene,
The ︰ 3 of 2 ︰ 1 are mixed to get solvent by volume for isophorone, repefral, count in parts by weight, by 20 parts of PVDF fluorine
The titania nanoparticles mixing that carbon resin, 45 parts of solvents, 15 parts of titanium dioxides and 20 parts of surfaces are modified, is placed in cooling dress
In the stirred tank put, with 1000r/min rotating speed, 30min is dispersed with stirring, obtains pre-dispersed raw material；Pre-dispersed raw material is added
It is ground in grinder, is ground to raw material particle size as 25 μm, controls temperature to obtain varnish at 20 DEG C in process of lapping, by weight
Number meter is measured, 20 parts of multi-walled carbon nanotubes are added in 100 parts of ethyl acetate, obtain mixed liquor, mixed liquor is placed in and divided at a high speed
Dissipate in machine, 18min is disperseed at a high speed with 7000r/min rotating speed, obtains CNT dispersion liquid；Count in parts by weight, by 70 parts
Varnish is mixed with 100 parts of CNT dispersion liquids, and after being placed in stirred tank with 600r/min rotating speed stirring 20min, reduction is stirred
Mix rotating speed is 300r/min, and 20 parts of hexamethylene diisocyanates are added into stirred tank, obtain self-cleaning fluorocarbon paint.
Example 2
210mL absolute ethyl alcohols are mixed with the perfluoro capryl triethoxysilane aqueous solution that 110mL mass fractions are 2%, obtain silicon
Oxygen alkane solution, siloxane solution pH to 3.1 is adjusted with the acetic acid that mass fraction is 60%, siloxane solution is poured into beaker
In, 23h is stirred with 310r/min rotating speed with magnetic stirring apparatus, the silicon fluoride solution hydrolyzed；Prepare mass concentration
For 4 mg/mL titanium dioxide alcohol mixeding liquid, by the silicon fluoride solution of titanium dioxide alcohol mixeding liquid and hydrolysis with volume ratio
For 4: 1 mixing, beaker is placed in, after being stirred 7.5h with magnetic stirring apparatus with 420r/min rotating speed, is placed in high speed centrifugation
11min is centrifuged with 4300r/min rotating speed in machine, upper liquid is removed, isolated lower sediment, lower sediment is put into
Design temperature is in 82 DEG C of vacuum drying chamber, dries 13h, obtains the titania nanoparticles of surface modification；By toluene,
The ︰ 3 of 2 ︰ 1 are mixed to get solvent by volume for isophorone, repefral, count in parts by weight, by 21 parts of PVDF fluorine
The titania nanoparticles mixing that carbon resin, 47 parts of solvents, 17 parts of titanium dioxides and 22 parts of surfaces are modified, is placed in cooling dress
In the stirred tank put, with 1100r/min rotating speed, 32min is dispersed with stirring, obtains pre-dispersed raw material；Pre-dispersed raw material is added
It is ground in grinder, is ground to raw material particle size as 27 μm, controls temperature to obtain varnish at 25 DEG C in process of lapping, by weight
Number meter is measured, 22 parts of multi-walled carbon nanotubes are added in 110 parts of ethyl acetate, obtain mixed liquor, mixed liquor is placed in and divided at a high speed
Dissipate in machine, 19min is disperseed at a high speed with 7200/min rotating speed, obtains CNT dispersion liquid；Count in parts by weight, it is clear by 75 parts
Paint mixes with 105 parts of CNT dispersion liquids, after being placed in stirred tank with 700r/min rotating speed stirring 22min, reduces stirring
Rotating speed is 350r/min, and 22 parts of hexamethylene diisocyanates are added into stirred tank, obtain self-cleaning fluorocarbon paint.
Example 3
220mL absolute ethyl alcohols are mixed with the perfluoro capryl triethoxysilane aqueous solution that 120mL mass fractions are 2%, obtain silicon
Oxygen alkane solution, siloxane solution pH to 3.3 is adjusted with the acetic acid that mass fraction is 60%, siloxane solution is poured into beaker
In, 24 h are stirred with 320r/min rotating speed with magnetic stirring apparatus, the silicon fluoride solution hydrolyzed；Prepare mass concentration
For 4 mg/mL titanium dioxide alcohol mixeding liquid, by the silicon fluoride solution of titanium dioxide alcohol mixeding liquid and hydrolysis with volume ratio
For 4: 1 mixing, beaker is placed in, after being stirred 8 h with magnetic stirring apparatus with 450r/min rotating speed, is placed in supercentrifuge
In 12min centrifuged with 4500r/min rotating speed, remove upper liquid, isolated lower sediment, lower sediment be put into and set
Constant temperature degree is in 85 DEG C of vacuum drying chamber, dries 14 h, obtains the titania nanoparticles of surface modification；By toluene,
The ︰ 3 of 2 ︰ 1 are mixed to get solvent by volume for isophorone, repefral, count in parts by weight, by 22 parts of PVDF fluorine
The titania nanoparticles mixing that carbon resin, 50 parts of solvents, 20 parts of titanium dioxides and 25 parts of surfaces are modified, is placed in cooling dress
In the stirred tank put, with 1300r/min rotating speed, 35min is dispersed with stirring, obtains pre-dispersed raw material；Pre-dispersed raw material is added
It is ground in grinder, is ground to raw material particle size as 30 μm, controls temperature to obtain varnish at 30 DEG C in process of lapping, by weight
Number meter is measured, 25 parts of multi-walled carbon nanotubes are added in 120 parts of ethyl acetate, obtain mixed liquor, mixed liquor is placed in and divided at a high speed
Dissipate in machine, 20min is disperseed at a high speed with 7500r/min rotating speed, obtains CNT dispersion liquid；Count in parts by weight, by 80 parts
Varnish is mixed with 110 parts of CNT dispersion liquids, and after being placed in stirred tank with 800r/min rotating speed stirring 25min, reduction is stirred
Mix rotating speed is 400r/min, and 25 parts of hexamethylene diisocyanates are added into stirred tank, obtain self-cleaning fluorocarbon paint.
Comparative example
With the self-cleaning fluorocarbon paint of Kunshan company production as a comparison case to self-cleaning fluorocarbon paint produced by the present invention and contrast
Self-cleaning fluorocarbon paint in example carries out performance detection, and testing result is as shown in table 1：
1st, method of testing：
Automatically cleaning effect method of testing：F-C paint in example 1~3 and comparative example is placed in lipophile and haze pollution sources
Air natural environment under some cycles, test pollution after coating appearance change；
Adhesive force test is detected using adherometer；
Contact angle test is detected using contact angle instrument.
Table 1
It can be seen from above-mentioned middle data, it is clean that self-cleaning fluorocarbon paint produced by the present invention throws away holding under lipophile and haze environment
Unchanged, adhesive force is low, has very strong automatical cleaning ability, and contact angle is high, has super-hydrophobic automatic cleaning power, has wide answer
Use prospect.
Claims (6)
1. a kind of preparation method of self-cleaning fluorocarbon paint, it is characterised in that specifically preparation process is：
（1）200~220mL absolute ethyl alcohols are mixed with 100~120mL perfluoro capryl triethoxysilane aqueous solution, obtain silicon
Oxygen alkane solution, siloxane solution pH is adjusted with acetic acid, siloxane solution is poured into beaker, mixed with magnetic stirrer,
The silicon fluoride solution hydrolyzed；
（2）Preparing titanium dioxide alcohol mixeding liquid, titanium dioxide alcohol mixeding liquid is mixed with the silicon fluoride solution hydrolyzed, is placed in
Beaker, after being mixed with magnetic stirrer, it is placed in supercentrifuge and centrifuges, removes upper liquid, isolated lower floor
Precipitation, lower sediment is put into vacuum drying chamber, is dried, and obtains the titania nanoparticles of surface modification；
（3）Toluene, isophorone, repefral are mixed to get solvent, counted in parts by weight, by 20~22 parts
The titania nanoparticles that PVDF fluorocarbon resins, 45~50 parts of solvents, 15~20 parts of titanium dioxides and 20~25 parts of surfaces are modified
Mixing, is placed in the stirred tank with cooling device, is dispersed with stirring to obtain pre-dispersed raw material；
（4）Pre-dispersed raw material is added in grinder and is ground, temperature is controlled in process of lapping at 20~30 DEG C, is obtained clear
Paint, is counted in parts by weight, and 20~25 parts of multi-walled carbon nanotubes are added in 100~120 parts of ethyl acetate, obtain mixed liquor, will
Mixed liquor, which is placed in high speed dispersor high speed, to be disperseed, and obtains CNT dispersion liquid；
（5）Count in parts by weight, 70~80 parts of varnish are mixed with 100~110 parts of CNT dispersion liquids, are placed in stirred tank
After stirring, speed of agitator is reduced, 20~25 parts of hexamethylene diisocyanates are added into stirred tank, obtain self-cleaning fluorocarbon
Paint.
A kind of 2. preparation method of self-cleaning fluorocarbon paint according to claim 1, it is characterised in that：Step（1）Described
The mass fraction of the perfluoro capryl triethoxysilane aqueous solution is 2%, and the mass fraction of acetic acid is 20%, and siloxanes is adjusted with acetic acid
PH value of solution is 3.0~3.3, and agitator speed of agitator is 300~320r/min, and it is 22~24 h to be stirred the time.
A kind of 3. preparation method of self-cleaning fluorocarbon paint according to claim 1, it is characterised in that：Step（2）Described
The mass concentration of titanium dioxide alcohol mixeding liquid is 4 mg/mL, and titanium dioxide alcohol mixeding liquid mixes with the silicon fluoride solution hydrolyzed
The volume ratio of conjunction is 4: 1, and magnetic stirrer rotating speed is 400~450r/min, and it is 7~8 h to be stirred the time, at a high speed
Centrifuge speed is 4200~4500r/min, and the centrifugation time is 10~12min, vacuum drying chamber design temperature is 80~
85 DEG C, drying time is 12~14 h.
A kind of 4. preparation method of self-cleaning fluorocarbon paint according to claim 1, it is characterised in that：Step（3）Described
Toluene, isophorone, the volume ratio of repefral mixing are the ︰ 3 of 2 ︰ 1, and the rotating speed of stirred tank is 1000~1300r/
Min, it is 30~35min to be dispersed with stirring the time.
A kind of 5. preparation method of self-cleaning fluorocarbon paint according to claim 1, it is characterised in that：Step（4）Described
Raw material particle size is 25~30 μm after grinding, and high speed dispersor rotating speed be 7000~7500r/min, high speed jitter time for 18~
20min。
A kind of 6. preparation method of self-cleaning fluorocarbon paint according to claim 1, it is characterised in that：Step（5）Described
Speed of agitator is 600~800r/min, and mixing time is 20~25min, and reduction speed of agitator is 300~400r/min.
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Application publication date: 20180126 |