CN106810991A - A kind of anti-oxidant hybrid microspheres grafting silicon composite coating and preparation method thereof - Google Patents
A kind of anti-oxidant hybrid microspheres grafting silicon composite coating and preparation method thereof Download PDFInfo
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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
- C09D151/00—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers
- C09D151/10—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers grafted on to inorganic materials
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
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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 invention discloses a kind of anti-oxidant hybrid microspheres grafting silicon composite coating, it is made up of the raw material of following weight parts：Ferric chloride hexahydrate 79, Iron dichloride tetrahydrate 10 12, citric acid 23, methacryloxypropyl trimethoxy silane 12, tetraethyl orthosilicate 100 130, hexafluorobutyl acrylate 57, azodiisobutyronitrile 0.1 0.4, antioxidant 1010 0.8 2, N methyl pyrrolidones 67, pentaerythrite 35, dibutyl tin laurate 0.6 1, dialkyl group is to biphenol 0.5 1, cresyl diphenyl phosphate 12, cellulose propionate 23, calcirm-fluoride 2.5 3, alkanolamide 0.1 0.2, absolute ethyl alcohol, appropriate dimethylformamide.The present invention add dialkyl group to biphenol, antioxidant 1010 etc. can be effective raising finished product coating antioxygenic property, improve finished product anti-corrosive properties and bin stability.
Description
Technical field
The present invention relates to technical field of coatings, more particularly to a kind of anti-oxidant hybrid microspheres grafting silicon composite coating and its system
Preparation Method.
Background technology
In recent years, the corrosion for suppressing copper and its alloy using corrosion inhibiter has obtained extensive research, azole compounds such as three
Azoles miaow or thiazole, it is considered to be the high-efficient corrosion inhibitor of copper in different mediums, right its inhibitory action are depended on, copper removal and its alloy
Outside bulk properties, the pH value also with solution is relevant, because the pH value of solution not only affects corrosion mechanism, corrosion product and suppression
Agent molecules, here it is many corrosion inhibiter are not one of the reason for corrosion mitigating effect is good in middle acid medium.Another important original
Cause, the intrinsic toxicity of azole compounds, potential risk is brought when as metal inhibitor to environment and human health, also there is text
Report is offered, benzothiazolyl mercaptan acid, imidazoles corrosion inhibiter has environment-friendly characteristic, but as the corrosion inhibiter of metallic copper
For, in the medium containing halide ion, its inhibition efficiency is remarkably decreased；
Many studies have shown that BTA is one of maximally effective corrosion inhibitor of copper, these researchs, in the solution of different pH value
In carry out, show forming thicker film in low ph value solution although trend, resulting Cu-BTA films are can more to ooze
Oxygen flow, and it in the film of the optimal formation of pH neutral is by forming cupric oxide on the film that provides as protection anticorrosion not to be
Surface, this shows the Cu-BTA topology convergence degree highests of most slow growth kinetics.One group of environment-friendly 4- first in the past
Base research imidazoles oneself through showing, they are good corrosion inhibiter.Although copper is in neutral chloride media in acid chloride medium
Their efficiency is very low.Therefore, it is necessary to improve corrosion mitigating effect of the corrosion inhibiter in acid and neutral chloride medium；
Additionally, suppressing the corrosion of copper, such as polypyridine and polyaniline using conducting polymer coating in copper substrate surfaces, conduction is poly-
The subject matter of compound coating is the water permeability of polymer coating and weak adhesion.Weak bond at metal/polymer interface is destroyed
The failure of coating structure or function will be caused, finally, irreversible corrosion and damage is caused in interface；
In sum, the technology such as the self-assembled film of copper, corrosion inhibiter, conducting polymer coating is served preferably to the inhibition aspect of copper
Effect, but still come with some shortcomings, such as the combination between self-assembled film and conducting polymer coating and metallic substrates interface
Power is low, pollution of the corrosion inhibiter to environment, therefore, how to develop a kind of efficient, low toxicity, environment-friendly copper anti-corrosion method turns into new
Research emphasis；
Because super hydrophobic surface has very important application prospect in theoretical research and practical application, therefore, super-hydrophobic solid
The structure on surface causes one of extensive concern, the study hotspot as materialogy in recent years and Surface Science field；
A key factor for influenceing surface of solids wellability is surface free energy, when surface free energy is reduced, hydrophobic performance
Will be increased.Even if however, with minimum surface can surface of smooth solid and water also only 119 ° of contact angle, because
This, only can not obtain super hydrophobic surface by drop low-surface-energy.Existing research shows, builds super hydrophobic surface and mainly pass through
Two approach:One is modifying low-surface energy substance in rough substrate surface;The second is built in hydrophobic surface having necessarily
The micro nano structure of roughness.According to this two approach, the method that scientists have developed many structure super hydrophobic surfaces builds
The super hydrophobic surface of different surfaces structures.Structure progress on super hydrophobic surface and its spun in building field, clothes
The summary in the fields such as field, biomedicine is knitted, oneself there are some documents to be summarized, it is contemplated that metal material faces in the environment
Etching problem, and super hydrophobic surface is one of very promising protecting metallic surface method；Because super-hydrophobic coat has
Unique surface property, such as self-cleaning, soil resistance, condensation-resistant etc., super hydrophobic surface are used for metal material, can play certainly
Cleaning, suppression surface corrosion and other effects.
The content of the invention
The object of the invention is exactly to make up the defect of prior art, there is provided a kind of anti-oxidant hybrid microspheres grafting silicon is combined
Coating and preparation method thereof.
The present invention is achieved by the following technical solutions：
A kind of anti-oxidant hybrid microspheres grafting silicon composite coating, it is made up of the raw material of following weight parts：
Ferric chloride hexahydrate 7-9, Iron dichloride tetrahydrate 10-12, citric acid 2-3, methacryloxypropyl trimethoxy
Silane 1-2, tetraethyl orthosilicate 100-130, hexafluorobutyl acrylate 5-7, azodiisobutyronitrile 0.1-0.4, antioxidant
10100.8-2,1-METHYLPYRROLIDONE 6-7, pentaerythrite 3-5, dibutyl tin laurate 0.6-1, dialkyl group are to biphenol
0.5-1, cresyl diphenyl phosphate 1-2, cellulose propionate 2-3, calcirm-fluoride 2.5-3, alkanolamide 0.1-0.2, anhydrous second
Alcohol, appropriate dimethylformamide.
A kind of described anti-oxidant hybrid microspheres are grafted the preparation method of silicon composite coating, comprise the following steps：
（1）Above-mentioned cellulose propionate is added in the deionized water of 20-30 times of its weight, is stirred, liter high-temperature is 56-
70 DEG C, above-mentioned alkanolamide is added, insulated and stirred 4-9 minutes, obtain acid amides dispersion liquid；
（2）Above-mentioned dialkyl group is added in the absolute ethyl alcohol of 30-40 times of its weight to biphenol, is stirred, rise high-temperature
It is 60-64 DEG C, adds above-mentioned antioxidant 1010, insulated and stirred 10-15 minutes, mix with above-mentioned acid amides dispersion liquid, stirs,
The 15-20% of above-mentioned tetraethyl orthosilicate weight is added, stirring reaction 1-2 hours, anti-oxidant colloidal sol is obtained；
（3）By above-mentioned ferric chloride hexahydrate, Iron dichloride tetrahydrate mix, be added to 100-140 times of compound weight go from
In sub- water, stir, it is the ammoniacal liquor of 6-9% to add concentration, and regulation pH is 11-12, is passed through nitrogen, and constant temperature is stirred at 80-85 DEG C
Mix 30-40 minutes, it is 90-95 DEG C to rise high-temperature, is incubated 1-2 hours, and suction filtration obtains filter cake；
（4）Above-mentioned filter cake is added in anti-oxidant colloidal sol, ultrasonic 3-4 minutes, filtering, by precipitation deionized water, anhydrous second
Alcohol is washed 2-3 times successively, is dried at 90-100 DEG C of vacuum 1-2 hours, is cooled to normal temperature, is added to going for 10-17 times of its weight
In ionized water, above-mentioned citric acid is added, it is ultrasonic 10-20 minutes, in feeding baking oven, dry completely, obtain sour modification magnetic fluid；
（5）Above-mentioned pentaerythrite is incubated 10-15 minutes at 76-80 DEG C, above-mentioned dibutyl tin laurate is added, stirring is equal
It is even, above-mentioned calcirm-fluoride, acid modification magnetic fluid are added, stirring to normal temperature adds above-mentioned 1-METHYLPYRROLIDONE, ultrasonic 1-2 minutes,
Filtering, precipitation absolute ethyl alcohol, deionized water is washed 2-3 times successively, air drying, obtains modified magnetic fluid；
（6）Above-mentioned modified magnetic fluid is taken, is added in 800-1000 times of its weight, 57-60% ethanol solution, ultrasonic 20-30
Minute, sequentially add above-mentioned cresyl diphenyl phosphate, methacryloxypropyl trimethoxy silane, remaining positive silicon
Acetoacetic ester, 700-800 revs/min is stirred 6-7 hour, suction filtration, by filter cake absolute ethanol washing 3-4 times, at 100-105 DEG C very
Sky is dried 20-25 hours, obtains ethenyl blocking compound particle；
（7）Above-mentioned ethenyl blocking magnetic particle is added in the dimethylformamide of 100-120 times of its weight, ultrasonic 50-
60 minutes, nitrogen is passed through, adds aforesaid propylene acid hexafluoro butyl ester, azodiisobutyronitrile, insulation reaction 6-7 is small at 70-80 DEG C
When, remaining each raw material is added, normal temperature is cooled to, suction filtration washes filter cake dimethylformamide 2-3 times, the vacuum at 76-80 DEG C
Dry 10-12 hours, obtain the coating.
Described a kind of anti-oxidant hybrid microspheres are grafted silicon composite coating, and the application method of the coating is：
Above-mentioned coating is added in the n- methyl pyrrolidones of 8-10 times of its weight, is stirred, be coated to what is cleaned up
Substrate surface, air drying, you can.
It is an advantage of the invention that：The present invention obtains magnetic and receives with ferric chloride hexahydrate, Iron dichloride tetrahydrate as presoma
Rice corpuscles is core, why can in ethanol have good dispersion stabilization with the magnetic nano-particle of citric acid modification, be because
It is that citric acid carboxyl and nanoparticle surface iron atom are chelated, and the carboxyl or hydroxyl that do not chelate are stretched in etoh solvent, so
The magnetic particle surface of the citric acid cladding for obtaining can show phase well for water-wet behavior with the reaction medium such as water, ethanol
Capacitive, then by methacryloxypropyl trimethoxy silane and the hydrolysis of tetraethyl orthosilicate, in magnetic particle table
Face introduces the siloxanes of ethenyl blocking, obtains the hybrid microspheres of ethenyl blocking, is lived for graft polymerization reaction provides vinyl
Property group, then with azo-bis-isobutyl cyanide as initiator, hexafluorobutyl acrylate is monomer, is successfully grafted on hybrid microspheres surface
Polyacrylic acid hexafluoro butyl ester polymer, obtains the organic inorganic hybridization particle of poly- fluorine carbon modification, then disperses hybrid particulates
To in n- methyl pyrrolidones, Copper base material surface is coated in, fluoropolymer segment reduces coating in the outside of compound particle
Surface can, so as to impart coating superhydrophobic characteristic；
The present invention add dialkyl group to biphenol, antioxidant 1010 etc. can be effective raising finished product coating inoxidizability
Can, improve the anti-corrosive properties and bin stability of finished product.
Specific embodiment
A kind of anti-oxidant hybrid microspheres grafting silicon composite coating, it is made up of the raw material of following weight parts：
Ferric chloride hexahydrate 7, Iron dichloride tetrahydrate 10, citric acid 2, methacryloxypropyl trimethoxy silane 1, just
Silester 100, hexafluorobutyl acrylate 5, azodiisobutyronitrile 0.1, antioxidant 1010 0.8, N methyl pyrrolidones 6, season penta
Tetrol 3, dibutyl tin laurate 0.6, dialkyl group to biphenol 0.5, cresyl diphenyl phosphate 1, cellulose propionate 2,
Calcirm-fluoride 2.5, alkanolamide 0.1, absolute ethyl alcohol, appropriate dimethylformamide.
A kind of described anti-oxidant hybrid microspheres are grafted the preparation method of silicon composite coating, comprise the following steps：
（1）Above-mentioned cellulose propionate is added in the deionized water of 20 times of its weight, is stirred, it is 56 DEG C to rise high-temperature,
Above-mentioned alkanolamide is added, insulated and stirred 4 minutes obtains acid amides dispersion liquid；
（2）Above-mentioned dialkyl group is added in the absolute ethyl alcohol of 30 times of its weight to biphenol, is stirred, it is 60 to rise high-temperature
DEG C, above-mentioned antioxidant 1010 is added, insulated and stirred 10 minutes mixes with above-mentioned acid amides dispersion liquid, stirs, and addition is above-mentioned just
The 15% of silester weight, stirring reaction 1 hour, obtains anti-oxidant colloidal sol；
（3）Above-mentioned ferric chloride hexahydrate, Iron dichloride tetrahydrate are mixed, the deionized water of 100 times of compound weight is added to
In, stir, the ammoniacal liquor that concentration is 6% is added, regulation pH is 11, is passed through nitrogen, and constant temperature is stirred 30 minutes at 80 DEG C, is risen
High-temperature is 90 DEG C, is incubated 1 hour, and suction filtration obtains filter cake；
（4）Above-mentioned filter cake is added in anti-oxidant colloidal sol, ultrasound 3 minutes, filtering, by precipitation deionized water, absolute ethyl alcohol
Wash 2 times successively, dried 1 hour at 90 DEG C of vacuum, be cooled to normal temperature, be added in the deionized water of 10 times of its weight, add
Above-mentioned citric acid, ultrasound 10 minutes in feeding baking oven, is dried completely, obtains sour modification magnetic fluid；
（5）Above-mentioned pentaerythrite is incubated 10 minutes at 76 DEG C, above-mentioned dibutyl tin laurate is added, stirred, plus
Enter above-mentioned calcirm-fluoride, acid modification magnetic fluid, stirring to normal temperature adds above-mentioned N methyl pyrrolidones, and ultrasonic 1 minute, filtering will
Precipitation absolute ethyl alcohol, deionized water are washed 2 times successively, and air drying obtains modified magnetic fluid；
（6）Take above-mentioned modified magnetic fluid, be added in 800 times of its weight, 57% ethanol solution, ultrasound 20 minutes, successively plus
Enter above-mentioned cresyl diphenyl phosphate, methacryloxypropyl trimethoxy silane, remaining tetraethyl orthosilicate, 700
Rev/min stirring 6 hours, suction filtration, by filter cake absolute ethanol washing 3 times, is vacuum dried 20 hours at 100 DEG C, obtains vinyl
End-blocking compound particle；
（7）Above-mentioned ethenyl blocking magnetic particle is added in the dimethylformamide of 100 times of its weight, ultrasound 50 minutes,
Nitrogen is passed through, aforesaid propylene acid hexafluoro butyl ester, azodiisobutyronitrile is added, insulation reaction 6 hours at 70 DEG C add remaining each
Raw material, is cooled to normal temperature, and suction filtration washes filter cake dimethylformamide 2 times, is vacuum dried 10 hours at 76 DEG C, obtains described
Coating.
Described a kind of anti-oxidant hybrid microspheres are grafted silicon composite coating, and the application method of the coating is：
Above-mentioned coating is added in the n methyl pyrrolidones of 8 times of its weight, is stirred, be coated to the base material for cleaning up
Surface, air drying, you can.
Performance test:
Contact angle is 154 ± 1.5.
Claims (3)
1. a kind of anti-oxidant hybrid microspheres are grafted silicon composite coating, it is characterised in that it is made up of the raw material of following weight parts
's：
Ferric chloride hexahydrate 7-9, Iron dichloride tetrahydrate 10-12, citric acid 2-3, methacryloxypropyl trimethoxy
Silane 1-2, tetraethyl orthosilicate 100-130, hexafluorobutyl acrylate 5-7, azodiisobutyronitrile 0.1-0.4, antioxidant
10100.8-2,1-METHYLPYRROLIDONE 6-7, pentaerythrite 3-5, dibutyl tin laurate 0.6-1, dialkyl group are to biphenol
0.5-1, cresyl diphenyl phosphate 1-2, cellulose propionate 2-3, calcirm-fluoride 2.5-3, alkanolamide 0.1-0.2, anhydrous second
Alcohol, appropriate dimethylformamide.
2. a kind of anti-oxidant hybrid microspheres as claimed in claim 1 are grafted the preparation method of silicon composite coating, it is characterised in that
Comprise the following steps：
（1）Above-mentioned cellulose propionate is added in the deionized water of 20-30 times of its weight, is stirred, liter high-temperature is 56-
70 DEG C, above-mentioned alkanolamide is added, insulated and stirred 4-9 minutes, obtain acid amides dispersion liquid；
（2）Above-mentioned dialkyl group is added in the absolute ethyl alcohol of 30-40 times of its weight to biphenol, is stirred, rise high-temperature
It is 60-64 DEG C, adds above-mentioned antioxidant 1010, insulated and stirred 10-15 minutes, mix with above-mentioned acid amides dispersion liquid, stirs,
The 15-20% of above-mentioned tetraethyl orthosilicate weight is added, stirring reaction 1-2 hours, anti-oxidant colloidal sol is obtained；
（3）By above-mentioned ferric chloride hexahydrate, Iron dichloride tetrahydrate mix, be added to 100-140 times of compound weight go from
In sub- water, stir, it is the ammoniacal liquor of 6-9% to add concentration, and regulation pH is 11-12, is passed through nitrogen, and constant temperature is stirred at 80-85 DEG C
Mix 30-40 minutes, it is 90-95 DEG C to rise high-temperature, is incubated 1-2 hours, and suction filtration obtains filter cake；
（4）Above-mentioned filter cake is added in anti-oxidant colloidal sol, ultrasonic 3-4 minutes, filtering, by precipitation deionized water, anhydrous second
Alcohol is washed 2-3 times successively, is dried at 90-100 DEG C of vacuum 1-2 hours, is cooled to normal temperature, is added to going for 10-17 times of its weight
In ionized water, above-mentioned citric acid is added, it is ultrasonic 10-20 minutes, in feeding baking oven, dry completely, obtain sour modification magnetic fluid；
（5）Above-mentioned pentaerythrite is incubated 10-15 minutes at 76-80 DEG C, above-mentioned dibutyl tin laurate is added, stirring is equal
It is even, above-mentioned calcirm-fluoride, acid modification magnetic fluid are added, stirring to normal temperature adds above-mentioned 1-METHYLPYRROLIDONE, ultrasonic 1-2 minutes,
Filtering, precipitation absolute ethyl alcohol, deionized water is washed 2-3 times successively, air drying, obtains modified magnetic fluid；
（6）Above-mentioned modified magnetic fluid is taken, is added in 800-1000 times of its weight, 57-60% ethanol solution, ultrasonic 20-30
Minute, sequentially add above-mentioned cresyl diphenyl phosphate, methacryloxypropyl trimethoxy silane, remaining positive silicon
Acetoacetic ester, 700-800 revs/min is stirred 6-7 hour, suction filtration, by filter cake absolute ethanol washing 3-4 times, at 100-105 DEG C very
Sky is dried 20-25 hours, obtains ethenyl blocking compound particle；
（7）Above-mentioned ethenyl blocking magnetic particle is added in the dimethylformamide of 100-120 times of its weight, ultrasonic 50-
60 minutes, nitrogen is passed through, adds aforesaid propylene acid hexafluoro butyl ester, azodiisobutyronitrile, insulation reaction 6-7 is small at 70-80 DEG C
When, remaining each raw material is added, normal temperature is cooled to, suction filtration washes filter cake dimethylformamide 2-3 times, the vacuum at 76-80 DEG C
Dry 10-12 hours, obtain the coating.
3. a kind of anti-oxidant hybrid microspheres according to claim 1 are grafted silicon composite coating, it is characterised in that the coating
Application method be：
Above-mentioned coating is added in the n- methyl pyrrolidones of 8-10 times of its weight, is stirred, be coated to what is cleaned up
Substrate surface, air drying, you can.
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Cited By (2)
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| CN108047584A (en) * | 2017-12-25 | 2018-05-18 | 桐城市祥泰塑业有限公司 | A kind of light-weight environment-friendly building plastic plate material and preparation method thereof |
| CN108997561A (en) * | 2018-07-11 | 2018-12-14 | 桐城市新瑞建筑工程有限公司 | A kind of methylation conductive micro-balloons and preparation method thereof |
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| CN105907226A (en) * | 2016-06-12 | 2016-08-31 | 合肥和安机械制造有限公司 | Metallic copper anti-corrosion hydrophobic coating and preparation method thereof |
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| CN106047030A (en) * | 2016-06-13 | 2016-10-26 | 合肥和安机械制造有限公司 | Resin-based metal copper anticorrosion coating and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108047584A (en) * | 2017-12-25 | 2018-05-18 | 桐城市祥泰塑业有限公司 | A kind of light-weight environment-friendly building plastic plate material and preparation method thereof |
| CN108997561A (en) * | 2018-07-11 | 2018-12-14 | 桐城市新瑞建筑工程有限公司 | A kind of methylation conductive micro-balloons and preparation method thereof |
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Application publication date: 20170609 |