CN109385154A - A kind of new green environment protection electrochemical protection film layer and its preparation process - Google Patents
A kind of new green environment protection electrochemical protection film layer and its preparation process Download PDFInfo
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
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Abstract
The invention belongs to technical field of composite materials, it is related to a kind of new green environment protection electrochemical protection film layer and its preparation process.The present invention mainly solves the deficiencies in the prior art; a kind of new green environment protection electrochemical protection film layer and its preparation process, the component including following mass percent: 10%~20% polyaniline, 20%~30% nano-titanium dioxide, 50%~70% PVB are provided.The present invention enables nanoparticle to be filled into the hole and defect of coating using dimensional effect, the skin effect etc. of titanium dioxide nano-particle, efficiently solve the problems, such as that poor polyaniline coating film forming, bad dispersibility, shielding are poor, to give full play to the antiseptic property of polyaniline coating.There are photoelectric nano-titanium dioxide and polyaniline to interact, the effect of photic cathodic protection can also be obtained, to further increase the antiseptic property of coating.
Description
Technical field
The invention belongs to technical field of composite materials, it is related to a kind of new green environment protection electrochemical protection film layer and its preparation
Technique.
Background technique
Metal erosion problem brings about great losses to national economy.In various preventive means, coating technology is because being applicable in model
Enclose wide, repairing is convenient and is widely used.In various coatings, metal coating often has peeling, bubbling, porosity big, shows thick
The problems such as rough, Inorganic and Nonmetallic Coating can make that nonuniform organization, there are hole and expensive, organic paintings due to technological problems
There is rotten, heat-resisting cold resistance difference easy to aging in layer.Therefore, the high anti-corrosion coating for developing new green environment protection is current gold
Belong to one of the target that corrosion and protection field is pursued.
Polyaniline (PANI) is because having easily prepared, higher conductivity, good chemical stability and unique doping
The features such as mechanism, it is considered to be one of most promising conducting polymer.De Berry in 1985 has found PANI to stainless for the first time
Steel has antisepsis, causes the extensive concern of domestic and foreign scholars.Although polyaniline anti-corrosion coating has unique scratch resistance
With the performance of anti-spot corrosion, but the problems such as there are shielding, dissolubility, poor film formings, it is not easy to use directly as coating.Research hair
Now addition nano particle can fill up the hole in polyaniline structure, enhance shielding action, obtain pattern, structure it is more fine and close,
Stable anticorrosive polyaniline coating.
Nano-titanium dioxide has very high chemical stability and thermal stability, and good dispersion, cheap and easy to get, frequently as
Filler grain and polymer etc. form composite material.In addition, titanium dioxide has unique photoelectric conversion effect, nanometer titanium dioxide
The photic cathodic protection coatings of titanium are the novel cathode protection techniques of Recent study.Under illumination, the excitation of titanium dioxide valence-band electrons
To conduction band, electron-hole pair is formed, electron-transport to metallic matrix makes metal potential drop down to the cathodic protection that do not corrode
Area realizes the protection to metal.
It in the prior art, is mostly to enable nanoparticle using dimensional effect, the skin effect etc. of titanium dioxide nano-particle
It is filled into the hole and defect of coating, improves coating compactness, to effectively improve the antiseptic property of coating, or modified
The photic cathodic protection of titanium dioxide acts on, and makes it have better photic cathodic protection effect.And it is prepared on metallic matrix
The coating of two kinds of materials of polyaniline and titanium dioxide, the technology for making the synergistic effect of two kinds of materials play protection to metal not yet mention
And.
Summary of the invention
The present invention mainly solves the deficiencies in the prior art, provides a kind of new green environment protection electrochemical protection film
Layer and its preparation process, the present invention enable nanoparticle to fill out using dimensional effect, the skin effect etc. of titanium dioxide nano-particle
It is charged in the hole and defect of coating, efficiently solves the problems, such as that poor polyaniline coating film forming, bad dispersibility, shielding are poor,
To give full play to the antiseptic property of polyaniline coating.There are photoelectric nano-titanium dioxide and polyaniline to interact, also
The effect of photic cathodic protection can be obtained, to further increase the antiseptic property of coating.
The technical scheme of the invention to solve the technical problem is: a kind of new green environment protection electrochemical protection film
Layer, which is characterized in that the component including following mass percent: 10%~20% polyaniline, 20%~30% nanometer two
Titanium oxide, 50%~70% PVB.
Further technical solution is that the structure of the protective film layer is polyaniline/PVB --- nano-titanium dioxide/PVB
Duplex coating.
Further technical solution is that the structure of the protective film layer is nano-titanium dioxide/PVB --- polyaniline/PVB
Duplex coating.
Further technical solution is, the structure of the protective film layer be polyaniline/nano-titanium dioxide/PVB uniformly more
Dissipate the composite coating of distribution.
A kind of preparation process of new green environment protection electrochemical protection film layer, comprising the following steps:
(1) acid solution is mixed with aniline monomer, ultrasound after in ice-water bath magnetic agitation；
(2) oxidant ammonium persulfate is mixed with acid solution, is added in the mixed liquor of magnetic agitation, it is quiet after the reaction was completed
It sets, filter, dry polyaniline powder after being rinsed with deionized water and ethyl alcohol；
(3) PVB dissolution is taken in methyl alcohol, magnetic agitation is ultrasonic again, obtains PVB slurry；
(4) polyaniline powder is put into after being ground in grinding alms bowl and a small amount of methanol is added stirs into slurry, which is added
It is stirred into PVB slurry, obtains the even composite coating of polyaniline/PVB；
(5) it is dried after polyaniline, PVB composite coating being coated in the metal surface handled well with knife coating, obtains polyphenyl
Amine/PVB composite coating；
(6) in methyl alcohol by PVB dissolution, magnetic agitation obtains PVB slurry；
(7) nano titanium dioxide powder is added in PVB slurry magnetic agitation after ultrasound, obtained in nanometer titanium dioxide
Titanium/PVB slurry；
(8) it is coated with polyaniline/PVB coated metallic plate and is put into nano-titanium dioxide/PVB slurry, using Best-Effort request
Method prepares nano-titanium dioxide/PVB coating.
A kind of preparation process of new green environment protection electrochemical protection film layer, comprising the following steps:
A, in methyl alcohol by PVB dissolution, magnetic agitation obtains PVB slurry；
B, nano titanium dioxide powder is added in PVB slurry magnetic agitation after ultrasound, obtain nano-titanium dioxide/
PVB slurry；
C, the metal plate handled well is put into nano-titanium dioxide/PVB slurry, nano-silica is prepared using dip-coating method
Change titanium/PVB coating；
D, acid solution is mixed with aniline monomer, ultrasound after in ice-water bath magnetic agitation, by oxidant ammonium persulfate and acid
Solution mixing, is added in the mixed liquor of magnetic agitation, stands, filters after the reaction was completed, does after being rinsed with deionized water and ethyl alcohol
It is dry；
E, PVB dissolution is taken in methyl alcohol, magnetic agitation is ultrasonic again, obtains PVB slurry；
F, polyaniline powder is put into after being ground in grinding alms bowl and a small amount of methanol is added stirs into slurry, which is added to
It is stirred in PVB slurry, obtains the finely dispersed composite coating of polyaniline, PVB；
G, compound coated with polyaniline/PVB is prepared using knife coating on nano-titanium dioxide/PVB coating metal plate
Coating.
A kind of preparation process of new green environment protection electrochemical protection film layer, comprising the following steps:
A, acid solution is mixed with aniline monomer, and titanium dioxide is added thereto, ultrasound after in ice-water bath magnetic agitation；
B, oxidant ammonium persulfate is mixed with acid solution, is added in the mixed liquor of magnetic agitation, stand after the reaction was completed,
Filtering, it is dry after being rinsed with deionized water and ethyl alcohol, obtain polyaniline/titanium dioxide composite powder；
C, polyaniline/titanium dioxide composite powder is put into after being ground in grinding alms bowl and a small amount of methanol stirring is added, starched
Material one；
D, PVB dissolution is taken in methyl alcohol, magnetic agitation is ultrasonic again, obtains slurry two；
E, slurry one and slurry two are mixed, obtain polyaniline/nano-titanium dioxide/PVB even dispersion distribution
Composite coating；
F, metal surface is polished smooth, is first cleaned by ultrasonic with deionized water, then rinsed and dried up with dehydrated alcohol；
G, metal plate is put into polyaniline/nano-titanium dioxide/PVB even dispersion distribution composite coating again, and used
Dip-coating method prepares polyaniline/nano-titanium dioxide/PVB even dispersion distribution composite coating in metal plate.
Further technical solution is, the acid solution is hydrochloric acid or sulfuric acid, and concentration is 1~2mol/L, volume is 100~
The mass ratio of 200mL, titanium dioxide and aniline is 2~10, APS and the mass ratio of the material of aniline is 0.5~1.5.
Further technical solution is that the bath temperature of ice-water bath is controlled at 0~5 DEG C, magnetic agitation in the step a
Between be 4~6h.
Further technical solution is that the mass ratio of methanol and PVB are 5~10 present invention with following in the step d
Advantage:
1, polyaniline, nano-titanium dioxide and PVB material used by the electrochemical protection film layer prepared by the present invention, it is honest and clean
Valence is easy to get, environmentally protective；
2, the electrochemical protection film layer production instrument equipment prepared by the present invention is simple, and technological operation is simple, condition
Controllably, it can reduce production cost；
3, the composite coating prepared by the present invention improves film forming, dispersibility and shielding, to give full play to polyaniline
The antiseptic property of coating；
4, the composite coating prepared by the present invention will have photoelectric nano-titanium dioxide and polyaniline to interact,
The effect that photic cathodic protection can be obtained further increases the antiseptic property of coating；
5, the photic cathodic protection that the composite coating prepared by the present invention is played the role of, with conventional cathode protection technique phase
Than the technology does not need consumption electric energy not only, and light anode can recycle, and be a kind of technology of green non-pollution.
Detailed description of the invention
Fig. 1 is the Cross Section Morphology of embodiment 1；
Fig. 2 is photoelectricity flow graph of the embodiment 1 in 3.5%NaCl；
Fig. 3 is photoelectricity bitmap of the embodiment 1 in 3.5%NaCl.
Specific embodiment
Below by embodiment, technical scheme of the present invention will be further explained in detail.
Embodiment 1
A kind of new green environment protection electrochemical protection film layer of the invention, which is characterized in that including following mass percent
Component: 10%~20% polyaniline, 20%~30% nano-titanium dioxide, 50%~70% PVB, structure are poly-
Aniline/PVB --- nano-titanium dioxide/PVB duplex coating.
Above-mentioned polyaniline/PVB --- nano-titanium dioxide/PVB duplex coating preparation process, comprising the following steps:
(1) the hydrochloric acid 90mL of 1M is taken to mix with 1mL aniline monomer, ultrasonic 30min dispersion, obtained mixed liquor is in ice-water bath
Magnetic agitation 30min in (controlled at 0C)；
(2) by 2.5g oxidant ammonium persulfate and 100mL mixed in hydrochloric acid, magnetic agitation is added with the speed of 1 drop per second
In mixed liquor, start timing after completion of dropwise addition, ice-water bath magnetic agitation stirs 4h, filters after standing 12h, with deionized water and second
Alcohol rinses, remove impurity and small-molecule substance respectively until filtrate be it is colourless, dry 12h is in 50 DEG C of baking oven to get green
Powder；
(3) 2gPVB is taken to be dissolved in 20mL methanol, ultrasound 2h again after magnetic agitation 6h obtains PVB slurry；
(4) polyaniline powder of 10wt% is put into grinding alms bowl and is ground, a small amount of methanol stirring is added in the sample after grinding
At slurry；
(5) slurry is added in PVB slurry and stirs 12h, obtain the finely dispersed polyaniline paint in PVB；
(6) preparation of titania coating is same as above；
(7) stainless steel surface is polished smooth, is first cleaned by ultrasonic with deionized water, then rinsed and dried up with dehydrated alcohol；
(8) titania coating is coated in the stainless steel surface handled well 1 time with the lifting of Best-Effort request technology, in room temperature
After lower drying, then polyaniline paint is dry on coating of titanium dioxide, being put into 50 DEG C of baking ovens with 10 microns of knife coating blade coating
4h。
Polyaniline/PVB that above-described embodiment 1 is prepared --- nano-titanium dioxide/PVB duplex coating Cross Section Morphology is such as
Shown in Fig. 1, the photoelectricity flow graph, photoelectricity bitmap in 3.5%NaCl are respectively as shown in Figures 2 and 3.
Embodiment 2
A kind of new green environment protection electrochemical protection film layer of the invention, which is characterized in that including following mass percent
Component: 10%~20% polyaniline, 20%~30% nano-titanium dioxide, 50%~70% PVB, structure be receive
Rice titanium dioxide/PVB --- polyaniline/PVB duplex coating.
Above-mentioned nano-titanium dioxide/PVB --- polyaniline/PVB duplex coating preparation process, comprising the following steps:
1) in methyl alcohol by PVB dissolution, magnetic agitation obtains PVB slurry；
2) nano titanium dioxide powder is added in PVB slurry magnetic agitation after ultrasound, obtain nano-titanium dioxide/
PVB slurry；
3) metal plate is put into nano-titanium dioxide/PVB slurry, nano-titanium dioxide/PVB is prepared using dip-coating method
Coating；
4) acid solution is mixed with aniline monomer, ultrasound after in ice-water bath magnetic agitation；
5) APS is mixed with acid solution, is added in the mixed liquor of magnetic agitation, after the reaction was completed stand, filter, spend from
Sub- water and ethyl alcohol are dry after rinsing；
6) PVB dissolution is taken in methyl alcohol, magnetic agitation is ultrasonic again, obtains PVB slurry；
7) polyaniline powder is put into after being ground in grinding alms bowl and a small amount of methanol is added stirs into slurry；
8) slurry is added in PVB slurry and is stirred, obtain the finely dispersed composite coating of polyaniline, PVB；
9) compound coated with polyaniline/PVB is prepared using knife coating on nano-titanium dioxide/PVB coating metal plate
Coating.
Embodiment 3
A kind of new green environment protection electrochemical protection film layer of the invention, which is characterized in that including following mass percent
Component: 10%~20% polyaniline, 20%~30% nano-titanium dioxide, 50%~70% PVB, structure are poly-
Aniline/nano-titanium dioxide/PVB even dispersion distribution composite coating.
The preparation process of above-mentioned polyaniline/nano-titanium dioxide/PVB even dispersion distribution composite coating, including it is following
Step:
A, acid solution is mixed with aniline monomer, and titanium dioxide is added thereto, ultrasound after in ice-water bath magnetic agitation；
B, oxidant ammonium persulfate is mixed with acid solution, is added in the mixed liquor of magnetic agitation, stand after the reaction was completed,
Filtering, it is dry after being rinsed with deionized water and ethyl alcohol, obtain polyaniline/titanium dioxide composite powder；
C, polyaniline/titanium dioxide composite powder is put into after being ground in grinding alms bowl and a small amount of methanol stirring is added, starched
Material one；
D, PVB dissolution is taken in methyl alcohol, magnetic agitation is ultrasonic again, obtains slurry two；
E, slurry one and slurry two are mixed, obtain polyaniline/nano-titanium dioxide/PVB even dispersion distribution
Composite coating；
F, metal plate is put into polyaniline/nano-titanium dioxide/PVB even dispersion distribution composite coating, and using leaching
Stain czochralski method prepares polyaniline/nano-titanium dioxide/PVB even dispersion distribution composite coating in metal plate.
Embodiment 4
Step 1: the preparation step of polyaniline/titanium dioxide nanocomposite:
It takes the hydrochloric acid 90mL of 1M to mix with 1mL aniline monomer, 4g titanium dioxide is added thereto, ultrasonic 30min dispersion obtains
The mixed liquor arrived magnetic agitation 30min in ice-water bath (controlled at 0 DEG C)；
By 2.5g oxidant ammonium persulfate and 100mL mixed in hydrochloric acid, the mixing of magnetic agitation is added with the speed of 1 drop per second
In liquid, start timing after completion of dropwise addition, ice-water bath magnetic agitation stirs 4h, filters after standing 12h, is rushed with deionized water and ethyl alcohol
Wash, remove impurity and small-molecule substance respectively until filtrate be it is colourless, dry 12h is in 50 DEG C of baking oven to get green powder；
Step 2: the preparation step of polyaniline/titanium dioxide nano composite dope:
2gPVB is taken to be dissolved in 20mL methanol, ultrasound 2h again after magnetic agitation 6h obtains PVB slurry；
The polyaniline/titanium dioxide powder of 10wt% is put into grinding alms bowl and is ground, a small amount of first is added in the sample after grinding
Alcohol stirs into slurry；
The slurry is added in PVB slurry and stirs 12h, the finely dispersed polyaniline/titanium dioxide in PVB is obtained and receives
Rice composite coating.
Step 3: the preparation step of anti-corrosive metal coating:
Stainless steel surface is polished smooth, is first cleaned by ultrasonic with deionized water, is then rinsed and is dried up with dehydrated alcohol；
Polyaniline/titanium dioxide nano composite dope is stainless coated in handling well with the lifting of Best-Effort request technology 1 time
Steel surface is put into 50 DEG C of baking ovens dry 4h after being dried at room temperature for.
The above is not intended to limit the present invention in any form, although the present invention is disclosed such as by embodiment
On, however, it is not intended to limit the invention, any person skilled in the art, is not departing from technical solution of the present invention range
It is interior, when the technology contents using the disclosure above make a little change or are modified to the equivalent embodiment of equivalent variations, but it is all
It is to the above embodiments according to the technical essence of the invention any simply to repair without departing from the content of technical solution of the present invention
Change, equivalent variations and modification, all of which are still within the scope of the technical scheme of the invention.
Claims (10)
1. a kind of new green environment protection electrochemical protection film layer, which is characterized in that the component including following mass percent: 10%
~20% polyaniline, 20%~30% nano-titanium dioxide, 50%~70% PVB.
2. a kind of new green environment protection electrochemical protection film layer according to claim 1, which is characterized in that the protective film
The structure of layer is polyaniline/PVB --- nano-titanium dioxide/PVB duplex coating.
3. a kind of new green environment protection electrochemical protection film layer according to claim 1, which is characterized in that the protective film
The structure of layer is nano-titanium dioxide/PVB --- polyaniline/PVB duplex coating.
4. a kind of new green environment protection electrochemical protection film layer according to claim 1, which is characterized in that the protective film
The structure of layer is polyaniline/nano-titanium dioxide/PVB even dispersion distribution composite coating.
5. a kind of preparation process of new green environment protection electrochemical protection film layer described in claim 2, which is characterized in that including with
Lower step:
(1) acid solution is mixed with aniline monomer, ultrasound after in ice-water bath magnetic agitation；
(2) oxidant ammonium persulfate is mixed with acid solution, is added in the mixed liquor of magnetic agitation, stood after the reaction was completed, mistake
Filter, dry polyaniline powder after being rinsed with deionized water and ethyl alcohol；
(3) PVB dissolution is taken in methyl alcohol, magnetic agitation is ultrasonic again, obtains PVB slurry；
(4) polyaniline powder is put into after being ground in grinding alms bowl and a small amount of methanol is added stirs into slurry, which is added to PVB
It is stirred in slurry, obtains the even composite coating of polyaniline/PVB；
(5) polyaniline, PVB composite coating are coated in knife coating it is dry behind the metal surface handled well, obtain polyaniline/
PVB composite coating；
(6) in methyl alcohol by PVB dissolution, magnetic agitation obtains PVB slurry；
(7) nano titanium dioxide powder is added in PVB slurry magnetic agitation after ultrasound, obtained in nano-titanium dioxide/PVB
Slurry；
(8) it is coated with polyaniline/PVB coated metallic plate and is put into nano-titanium dioxide/PVB slurry, using Best-Effort request legal system
Standby nano-titanium dioxide/PVB coating.
6. a kind of preparation process of new green environment protection electrochemical protection film layer described in claim 3, which is characterized in that including with
Lower step:
A, in methyl alcohol by PVB dissolution, magnetic agitation obtains PVB slurry；
B, nano titanium dioxide powder is added in PVB slurry magnetic agitation after ultrasound, obtained in nano-titanium dioxide/PVB
Slurry；
C, the metal plate handled well is put into nano-titanium dioxide/PVB slurry, nanometer titanium dioxide is prepared using dip-coating method
Titanium/PVB coating；
D, acid solution is mixed with aniline monomer, ultrasound after in ice-water bath magnetic agitation, by oxidant ammonium persulfate and acid solution
Mixing, is added in the mixed liquor of magnetic agitation, stands, filters after the reaction was completed, dry after being rinsed with deionized water and ethyl alcohol；
E, PVB dissolution is taken in methyl alcohol, magnetic agitation is ultrasonic again, obtains PVB slurry；
F, polyaniline powder is put into after being ground in grinding alms bowl and a small amount of methanol is added stirs into slurry, which is added to PVB
It is stirred in slurry, obtains the finely dispersed composite coating of polyaniline, PVB；
G, polyaniline/PVB composite coating is prepared using knife coating on being coated with nano-titanium dioxide/PVB coating metal plate.
7. a kind of preparation process of new green environment protection electrochemical protection film layer described in claim 4, which is characterized in that including with
Lower step:
A, acid solution is mixed with aniline monomer, and titanium dioxide is added thereto, ultrasound after in ice-water bath magnetic agitation；
B, oxidant ammonium persulfate is mixed with acid solution, is added in the mixed liquor of magnetic agitation, stood after the reaction was completed, mistake
Filter, it is dry after being rinsed with deionized water and ethyl alcohol, obtain polyaniline/titanium dioxide composite powder；
C, polyaniline/titanium dioxide composite powder is put into after being ground in grinding alms bowl and a small amount of methanol stirring is added, obtain slurry one；
D, PVB dissolution is taken in methyl alcohol, magnetic agitation is ultrasonic again, obtains slurry two；
E, slurry one and slurry two are mixed, it is compound obtains polyaniline/nano-titanium dioxide/PVB even dispersion distribution
Coating；
F, metal surface is polished smooth, is first cleaned by ultrasonic with deionized water, then rinsed and dried up with dehydrated alcohol；
G, metal plate is put into polyaniline/nano-titanium dioxide/PVB even dispersion distribution composite coating again, and using dipping
Czochralski method prepares polyaniline/nano-titanium dioxide/PVB even dispersion distribution composite coating in metal plate.
8. a kind of preparation process of new green environment protection electrochemical protection film layer according to claim 7, which is characterized in that
The acid solution is hydrochloric acid or sulfuric acid, and concentration is 1~2mol/L, and volume is 100~200mL, the quality of titanium dioxide and aniline
It is 0.5~1.5 than the mass ratio of the material for 2~10, APS and aniline.
9. a kind of preparation process of new green environment protection electrochemical protection film layer according to claim 7, which is characterized in that institute
The bath temperature control of ice-water bath in step a is stated at 0~5 DEG C, the magnetic agitation time is 4~6h.
10. novel intelligent electrochemical protection film layer and its preparation process according to claim 9, which is characterized in that the step
The mass ratio of methanol and PVB are 5~10 in rapid d.
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| CN116751495A (en) * | 2023-06-05 | 2023-09-15 | 吉林大学 | Self-repairing anti-corrosion and anti-fouling multifunctional coating |
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| CN1752160A (en) * | 2005-09-29 | 2006-03-29 | 武汉理工大学 | Phosphoric acid doped polyphenylamine phosphate priming paint and preparing process thereof |
| CN103540204A (en) * | 2012-07-17 | 2014-01-29 | 泰克大洋工业株式会社 | Anti-corrosive coating composition precursor |
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| CN116751495A (en) * | 2023-06-05 | 2023-09-15 | 吉林大学 | Self-repairing anti-corrosion and anti-fouling multifunctional coating |
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| CN109385154B (en) | 2021-01-05 |
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