CN107201140A - A kind of self-healing coatings and preparation method thereof - Google Patents
A kind of self-healing coatings and preparation method thereof Download PDFInfo
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- CN107201140A CN107201140A CN201710460466.3A CN201710460466A CN107201140A CN 107201140 A CN107201140 A CN 107201140A CN 201710460466 A CN201710460466 A CN 201710460466A CN 107201140 A CN107201140 A CN 107201140A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
Abstract
The present invention relates to a kind of self-healing coatings and preparation method thereof, belong to metal protection technical field.Homemade mesoporous silicon dioxide nano microballoon is added in BTA ethanol solution and stirred by the present invention, the mesoporous silicon dioxide nano microballoon of corrosion inhibiter must be loaded, the mesoporous silicon dioxide nano microballoon for loading corrosion inhibiter is added again and is stirred in zirconium-n-propylate ethanol solution, and filtered after adding salpeter solution stirring, obtain filter residue, filter residue is added in chitosan solution, sediment is centrifuged to obtain after ultrasonic disperse, sediment is added in sodium alginate soln, centrifuged after ultrasonic disperse, obtain and encapsulate corrosion inhibiter layer by layer, finally by epoxy resin, diluent, curing agent, corrosion inhibiter is encapsulated layer by layer, dispersant, ultrasonic disperse after stirring, obtain self-healing coatings.Of the invention with preparing, simple, load capacity is big and corrosion inhibiter discharges response function, has good repair ability for being damaged as the coating corrosion caused by natural environment.
Description
Technical field
The present invention relates to a kind of self-healing coatings and preparation method thereof, belong to metal protection technical field.
Background technology
In recent years, the validity of metal coating is carried out into common recognition using organic coating, it is considered that, organic coating is to gold
The protective effect of category matrix is mainly manifested in coating to water and the iris action of other aggressivity particles, also special pigment, tune
Inhibition, passivation, cathodic protection and the coating of material and the effect of metal surface cohesive force, but the erosion of natural environment and coating
Breakage caused by defect is can hardly be avoided, and aggressivity particle can reach coating/basal body interface through these defects, ultimately result in
Coating failure.The appearance of self-healing coatings provides the approach of reality for the long-effective protection and reduction coating frequency of maintenance of metal,
Self-healing coatings are exactly that after the integrality of coating is destroyed, its own can produce response to outside stimulus, by certain
Mode repairs damaged part, so as to recover protective value of the coating to matrix.To realize the self-repair function of coating, using organic
Coating protection metal is a kind of effective ways of prevention metal erosion.
To realize the self-repair function of coating, there are a kind of self-healing coatings based on microcapsules technology, this method is by inhibition
Agent is directly added into sol-gel intermediate layer, then nature loss unavoidably occurs for corrosion inhibiter, for as caused by natural environment
Then effect is limited for holiday, because the corrosion damage occurred under natural environment, it is difficult to which generation can make microcapsules in coating
The outside stimulus of rupture, and it is unable to reach selfreparing effect.
It would therefore be highly desirable to find a kind of self-healing coatings good to corrosion damage repairing effect caused by natural environment.
The content of the invention
The technical problems to be solved by the invention:Occur for traditional microcapsules self-healing coatings under natural environment
There is provided a kind of self-healing coatings and preparation method thereof for the problem of corrosion damage repairing effect is poor.
In order to solve the above technical problems, the technical solution adopted by the present invention is:
A kind of self-healing coatings, including epoxy resin, diluent, curing agent, corrosion inhibiter, dispersant, it is characterised in that described slow
Erosion agent is to encapsulate corrosion inhibiter layer by layer.
The epoxy resin is one kind in E-44, E-51, E-57.
The diluent is one or both of n-butanol, dimethylbenzene, acetone.
The curing agent is polyamide.
The dispersant is dispersant B YK-180.
The encapsulation corrosion inhibiter layer by layer is bag after the mesoporous silicon dioxide nano micro-spheres zirconia layer of load corrosion inhibiter
Chitosan layer is covered, then coats sodium alginate layer and is made.
The specific preparation process of self-healing coatings is:
S1. mesoporous silicon dioxide nano microballoon is prepared;
S2. by mesoporous silicon dioxide nano microballoon add mass fraction be 12% BTA ethanol solution in, in 10~50kPa
2~3h of lower stirring, stands and low pressure stirring standing centrifugally operated is repeated after centrifugation 2~3 times, must load the meso-porous titanium dioxide of corrosion inhibiter
Silicon nanoparticle;
S3. by load corrosion inhibiter mesoporous silicon dioxide nano microballoon add mass fraction be 2% zirconium-n-propylate ethanol solution in,
20~30min is stirred at 40~50 DEG C, mass fraction is added for 3% salpeter solution, is filtered after 1~2h of stirring, obtains filter residue,
Filter residue is added into mass fraction in 0.2~0.3% chitosan solution, to centrifuge to obtain sediment after ultrasonic disperse, then will precipitation
Thing adds mass fraction in 0.2~0.3% sodium alginate soln, to centrifuge after 15~20min of ultrasonic disperse, obtain and seal layer by layer
Fill corrosion inhibiter.
S4. count by weight, take 50~80 parts of epoxy resin, 20~40 parts of diluents, 25~40 parts of curing agent, 1~3
Part encapsulates corrosion inhibiter layer by layer, 1~2 part of dispersant, and 5~10min of ultrasonic disperse, obtains self-healing coatings after stirring.
The BTA ethanol solution is 10~30 times of mesoporous silicon dioxide nano microspheres quality.
The zirconium-n-propylate ethanol solution is 10~30 times of the mesoporous silicon dioxide nano microspheres quality of load corrosion inhibiter,
The chitosan solution is 30~60 times of the mesoporous silicon dioxide nano microspheres quality of load corrosion inhibiter, and the sodium alginate is molten
Liquid is 150~180 times that chitosan solution is the mesoporous silicon dioxide nano microspheres quality for loading corrosion inhibiter.
The present invention is compared with other method, and advantageous effects are:
(1)The present invention is using the high surface area, the mesoporous silicon dioxide nano micro-ball load corrosion inhibiter of big pore volume prepared, then leads to
Layer-by-layer is crossed, by zirconium oxide, chitosan, sodium alginate composition polyelectrolyte layer encapsulation corrosion inhibiter, and polyelectrolyte
Layer preferably, is conducive to encapsulating corrosion inhibiter in the coating scattered layer by layer, while passing through polyelectrolyte layer with epoxy resin compatibility
Energy sense temperature, pressure, pH value and coating localized variation simultaneously discharge sustained release agent, in fault location again film forming.
(2)The present invention, which has, prepares that simple, load capacity is big and corrosion inhibiter release-response function, for by natural environment
Caused coating corrosion damage has good repair ability.
Embodiment
0.50~0.75g cetyl trimethylammonium bromides are taken, adds in 200~300mL deionized waters and is well mixed, then
It is 8% sodium hydroxide solution to add 1.5~3.0mL mass fractions, at 70~80 DEG C, and 1~2h is stirred with 300~400r/min,
2.5~4.0mL tetraethyl orthosilicates are added dropwise with 0.1~0.2mL/min again, with 500~600r/min, 1~2h of insulated and stirred, filtering
Presoma is obtained, is 5% salt acid elution presoma 3~5 times with mass fraction, obtains pretreatment presoma;0.50~0.75g is taken to locate in advance
Presoma is managed, 5.0~7.5mL mass fractions are 37% hydrochloric acid, add in 100~150mL isopropanols, are incubated at 60~65 DEG C
4~5h is reacted, filter cake is filtered to obtain, filter cake is washed with deionized water and methanol 5~8 times, then the filter cake after washing is placed in vacuum
In drying box, dried at 30~40 DEG C to constant weight, obtain mesoporous silicon dioxide nano microballoon;Take the mesoporous dioxies of 0.50~0.75g
SiClx nanoparticle is added during 10~15mL mass fractions are 12% BTA ethanol solution, under 10~50kPa, with 500~
600r/min stirs 2~3h, then is placed in vacuum tank 1~2h of standing, and then centrifuging to precipitate, precipitation is added 10~
15mL mass fractions are repeatedly low pressure stirring standing centrifugally operated 2~3 times in 12% BTA ethanol solution, obtain load inhibition
The mesoporous silicon dioxide nano microballoon of agent;Take 0.50~0.75g to load the mesoporous silicon dioxide nano microballoon of corrosion inhibiter, add 10
~15mL mass fractions be 2% zirconium-n-propylate ethanol solution in, at 40~50 DEG C with 300~400r/min stirring 20~
30min, adds 3~5mL mass fractions for 3% salpeter solution, continues to stir after 1~2h and filters, obtains filter residue;Filter residue is added
25~30mL mass fractions be 0.2~0.3% chitosan solution in, to centrifuge and must sink after 15~20min of 300W ultrasonic disperses
Starch, then sediment is added during 75~100mL mass fractions are 0.2~0.3% sodium alginate soln, with 300W ultrasonic disperses
15~20min, then centrifuge to encapsulate corrosion inhibiter layer by layer;Count by weight, take 50~80 parts of epoxy resin E-44s, 10~
20 parts of n-butanols, 10~20 parts of dimethylbenzene, 25~40 parts of polyamide, 1~3 part encapsulates corrosion inhibiter, 1~2 part of dispersant layer by layer
BYK-180, stirs 5~10min of ultrasonic disperse after 5~10min with 100~200r/min, obtains self-healing coatings.
Example 1
0.75g cetyl trimethylammonium bromides are taken, adds in 300mL deionized waters and is well mixed, 3.0mL mass point is added
Number is 8% sodium hydroxide solution, at 80 DEG C, stirs 2h with 400r/min, then the positive silicic acid second of 4.0mL is added dropwise with 0.2mL/min
Ester, with 600r/min insulated and stirred 2h, filters to obtain presoma, is 5% salt acid elution presoma 5 times with mass fraction, must pre-process
Presoma;0.75g is taken to pre-process presoma, 7.5mL mass fractions are 37% hydrochloric acid, are added in 150mL isopropanols, at 65 DEG C
Insulation reaction 5h, filters to obtain filter cake, filter cake is washed with deionized water and methanol 8 times, then the filter cake after washing is placed in into vacuum done
In dry case, dried at 40 DEG C to constant weight, obtain mesoporous silicon dioxide nano microballoon;Take 0.75g mesoporous silicon dioxide nano microballoons
15mL mass fractions are added in 12% BTA ethanol solution, under 50kPa, to stir 3h with 600r/min, then be placed in vacuum
2h is stood in case, then centrifuging to precipitate, precipitation is added into 15mL mass fractions in 12% BTA ethanol solution
Repeat low pressure stirring and stand centrifugally operated 3 times, the mesoporous silicon dioxide nano microballoon of corrosion inhibiter must be loaded;0.75g is taken to load again
The mesoporous silicon dioxide nano microballoon of corrosion inhibiter, is added during 15mL mass fractions are 2% zirconium-n-propylate ethanol solution, at 50 DEG C
30min is stirred with 400r/min, 5mL mass fractions are added for 3% salpeter solution, continues to stir after 2h and filters, obtain filter residue;Will
Filter residue is added during 30mL mass fractions are 0.3% chitosan solution, to centrifuge to obtain sediment after 300W ultrasonic disperses 20min,
Sediment is added during 100mL mass fractions are 0.3% sodium alginate soln again, with 300W ultrasonic disperse 20min, then centrifuged point
Corrosion inhibiter is encapsulated layer by layer from obtaining;Count by weight, take 80 parts of epoxy resin E-44s, 20 parts of n-butanols, 20 parts of dimethylbenzene, 40 parts
Polyamide, 3 parts encapsulate corrosion inhibiter layer by layer, and 2 parts of dispersant B YK-180 stir ultrasonic disperse 10min after 10min with 200r/min,
Obtain self-healing coatings.
Example 2
0.50g cetyl trimethylammonium bromides are taken, adds in 200mL deionized waters and is well mixed, 1.5mL mass point is added
Number is 8% sodium hydroxide solution, at 70 DEG C, stirs 1h with 300r/min, then the positive silicic acid second of 2.5mL is added dropwise with 0.1mL/min
Ester, with 500r/min insulated and stirred 1h, filters to obtain presoma, is 5% salt acid elution presoma 3 times with mass fraction, must pre-process
Presoma;0.50g is taken to pre-process presoma, 5.0mL mass fractions are 37% hydrochloric acid, are added in 100mL isopropanols, at 60 DEG C
Insulation reaction 4h, filters to obtain filter cake, filter cake is washed with deionized water and methanol 5 times, then the filter cake after washing is placed in into vacuum done
In dry case, dried at 30 DEG C to constant weight, obtain mesoporous silicon dioxide nano microballoon;Take 0.50g mesoporous silicon dioxide nano microballoons
10mL mass fractions are added in 12% BTA ethanol solution, under 10kPa, to stir 2h with 500r/min, then be placed in vacuum
1h is stood in case, then centrifuging to precipitate, precipitation is added into 10mL mass fractions in 12% BTA ethanol solution
Repeat low pressure stirring and stand centrifugally operated 2 times, the mesoporous silicon dioxide nano microballoon of corrosion inhibiter must be loaded;Take 0.50g loads slow
Lose the mesoporous silicon dioxide nano microballoon of agent, add during 10mL mass fractions are 2% zirconium-n-propylate ethanol solution, at 40 DEG C with
300r/min stirs 20min, adds 3mL mass fractions for 3% salpeter solution, continues to stir after 1h and filters, obtains filter residue;Will filter
Slag is added during 25mL mass fractions are 0.2% chitosan solution, to centrifuge to obtain sediment after 300W ultrasonic disperses 15min, then
Sediment is added 75mL mass fractions in 0.2% sodium alginate soln, with 300W ultrasonic disperse 15min, then to centrifuge
Corrosion inhibiter is encapsulated layer by layer;Count by weight, take 50 parts of epoxy resin E-51,20 parts of dimethylbenzene, 25 parts of polyamide, 1 part is layer by layer
Corrosion inhibiter is encapsulated, 1 part of dispersant B YK-180, with ultrasonic disperse 5min after 100r/min stirrings 5min, obtains self-healing coatings.
Example 3
0.65g cetyl trimethylammonium bromides are taken, adds in 250mL deionized waters and is well mixed, 2.5mL mass point is added
Number is 8% sodium hydroxide solution, at 75 DEG C, stirs 2h with 350r/min, then the positive silicic acid second of 3.0mL is added dropwise with 0.1mL/min
Ester, with 550r/min insulated and stirred 1h, filters to obtain presoma, is 5% salt acid elution presoma 4 times with mass fraction, must pre-process
Presoma;0.62g is taken to pre-process presoma, 6.5mL mass fractions are 37% hydrochloric acid, are added in 130mL isopropanols, at 62 DEG C
Insulation reaction 4h, filters to obtain filter cake, filter cake is washed with deionized water and methanol 7 times, then the filter cake after washing is placed in into vacuum done
In dry case, dried at 35 DEG C to constant weight, obtain mesoporous silicon dioxide nano microballoon;Take 0.62g mesoporous silicon dioxide nano microballoons
12mL mass fractions are added in 12% BTA ethanol solution, under 40kPa, to stir 2h with 550r/min, then be placed in vacuum
1h is stood in case, then centrifuging to precipitate, precipitation is added into 12mL mass fractions in 12% BTA ethanol solution
Repeat low pressure stirring and stand centrifugally operated 3 times, the mesoporous silicon dioxide nano microballoon of corrosion inhibiter must be loaded;Take 0.60g loads slow
Lose the mesoporous silicon dioxide nano microballoon of agent, add during 12mL mass fractions are 2% zirconium-n-propylate ethanol solution, at 45 DEG C with
350r/min stirs 25min, adds 4mL mass fractions for 3% salpeter solution, continues to stir after 1h and filters, obtains filter residue;Will filter
Slag is added during 27mL mass fractions are 0.2% chitosan solution, to centrifuge to obtain sediment after 300W ultrasonic disperses 17min, then
Sediment is added 80mL mass fractions in 0.2% sodium alginate soln, with 300W ultrasonic disperse 17min, then to centrifuge
Corrosion inhibiter is encapsulated layer by layer;Count by weight, take 70 parts of epoxy resin E-57,15 parts of n-butanols, 150 parts of acetone, 30 parts of polyamides
Amine, 2 parts encapsulate corrosion inhibiter layer by layer, 1 part of dispersant B YK-180, with ultrasonic disperse 7min after 150r/min stirrings 7min, derived from repairing
Overcoating material.
Reference examples:The self-healing coatings of microcapsules technology
The application of coating:Select 1cm × 2cm × 0.2cm steel disc as experiment base material, carried out after grinding process, put with sand paper
Enter and be cleaned by ultrasonic 8min in acetone, dry after terminating, example 1 to example 3 and reference examples self-healing coatings are coated on after drying
Substrate surface, control coating thickness be 65 μm, coating terminate after, dry.
Base material after application is detected, examination criteria or method are as follows:
Pencil hardness:According to standard GB/T 6739-1996 method of testing, the pencil of coating is measured using small handcart
Hardness, pencil hardness of the hardness after coating when surface leaves the marking as coating is streaked using pencil.
Impact strength:Impact strength test is carried out according to standard GB/T 1732-1993.Instrument used in test
It is Du Pont's impact test machine, counterweight weight lkg.In test, counterweight is freely fallen from certain altitude, and taking occurs without out coating
Split, the maximum height of obscission is the impact strength of coating, unit is cmkg.
Self-reparing capability:Using the self-reparing capability of salt mist tester testing coating, use quality fraction is 5% during test
Sodium chloride solution, coating surface is sprayed on mist, control experimental temperature be 35 DEG C, spray time 170h.
Test result such as table 1.
Table 1
Detection project | Example 1 | Example 2 | Example 3 | Reference examples |
Pencil hardness(H) | 5H | 6H | 5H | 3H |
Impact strength(cm·kg) | 35 | 37 | 36 | 24 |
Self-reparing capability | Do not occur corrosion phenomenon | Do not occur corrosion phenomenon | Do not occur corrosion phenomenon | Coating surface has rust staining |
As shown in Table 1, the self-healing coatings hardness and impact strength that prepared by the present invention are high, while in salt spray test, not occurring
The phenomenons such as rust staining, embody it with higher self-reparing capability.
Claims (10)
1. a kind of self-healing coatings, including epoxy resin, diluent, curing agent, corrosion inhibiter, dispersant, it is characterised in that described
Corrosion inhibiter is to encapsulate corrosion inhibiter layer by layer.
2. a kind of self-healing coatings as claimed in claim 1, it is characterised in that the epoxy resin is E-44, E-51, E-57
In one kind.
3. a kind of self-healing coatings as claimed in claim 1, it is characterised in that the diluent is n-butanol, dimethylbenzene, third
One or both of ketone.
4. a kind of self-healing coatings as claimed in claim 1, it is characterised in that the curing agent is polyamide.
5. a kind of self-healing coatings as claimed in claim 1, it is characterised in that the dispersant is dispersant B YK-180.
6. a kind of self-healing coatings as claimed in claim 1, it is characterised in that the encapsulation corrosion inhibiter layer by layer is load inhibition
Chitosan layer is coated after the mesoporous silicon dioxide nano micro-spheres zirconia layer of agent, then coats sodium alginate layer and is made.
7. the preparation method of a kind of self-healing coatings as described in any one of claim 1~6, it is characterised in that review one's lessons by oneself overcoating
Material specific preparation process be:
S1. mesoporous silicon dioxide nano microballoon is prepared;
S2. by mesoporous silicon dioxide nano microballoon add mass fraction be 12% BTA ethanol solution in, in 10~50kPa
2~3h of lower stirring, stands and low pressure stirring standing centrifugally operated is repeated after centrifugation 2~3 times, must load the meso-porous titanium dioxide of corrosion inhibiter
Silicon nanoparticle;
S3. by load corrosion inhibiter mesoporous silicon dioxide nano microballoon add mass fraction be 2% zirconium-n-propylate ethanol solution in,
20~30min is stirred at 40~50 DEG C, mass fraction is added for 3% salpeter solution, is filtered after 1~2h of stirring, obtains filter residue,
Filter residue is added into mass fraction in 0.2~0.3% chitosan solution, to centrifuge to obtain sediment after ultrasonic disperse, then will precipitation
Thing adds mass fraction in 0.2~0.3% sodium alginate soln, to centrifuge after 15~20min of ultrasonic disperse, obtain and seal layer by layer
Fill corrosion inhibiter.
8. counting by weight, 50~80 parts of epoxy resin, 20~40 parts of diluents, 25~40 parts of curing agent, 1~3 part of layer are taken
Layer encapsulation corrosion inhibiter, 1~2 part of dispersant, 5~10min of ultrasonic disperse, obtains self-healing coatings after stirring.
9. a kind of self-healing coatings as claimed in claim 7, it is characterised in that the BTA ethanol solution is mesoporous two
10~30 times of silica nanoparticle quality.
10. a kind of self-healing coatings as claimed in claim 7, it is characterised in that the zirconium-n-propylate ethanol solution is load
10~30 times of the mesoporous silicon dioxide nano microspheres quality of corrosion inhibiter, the chitosan solution is mesoporous the two of load corrosion inhibiter
30~60 times of silica nanoparticle quality, the sodium alginate soln is that chitosan solution is load corrosion inhibiter mesoporous two
150~180 times of silica nanoparticle quality.
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