CN105131790B - Magnesium stearate is modified the preparation method of magnesium powder richness magnesium priming paint - Google Patents
Magnesium stearate is modified the preparation method of magnesium powder richness magnesium priming paint Download PDFInfo
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- CN105131790B CN105131790B CN201510617105.6A CN201510617105A CN105131790B CN 105131790 B CN105131790 B CN 105131790B CN 201510617105 A CN201510617105 A CN 201510617105A CN 105131790 B CN105131790 B CN 105131790B
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Abstract
The present invention relates to rich magnesium priming paint, specifically a kind of magnesium stearate is modified the preparation method of magnesium powder richness magnesium priming paint.Magnesium powder is modified to obtain magnesium stearate by the way that magnesium powder is dispersed in the butyl acetate solution of magnesium stearate and is stirred, this is modified magnesium powder to prepare rich magnesium priming paint.The inventive method can reduce magnesium powder reaction speed during cathodic protection in the case where not changing magnesium powder surface primary morphology and composition, extend the service life of rich magnesium priming paint, will play significant role in corrosion-resistant fields such as aviation, ocean engineerings.
Description
Technical field
The present invention relates to rich magnesium priming paint, specifically a kind of magnesium stearate is modified the preparation method of magnesium powder richness magnesium priming paint.
Background technology
Rich magnesium priming paint corrosion protection as Trend of Chrome-free corrosion protection technology substitute technology in the especially aviation of many fields
Field has wide practical use.Corrosion protection of the rich magnesium priming paint to aluminium alloy is a kind of electrochemical cathodic protection of sacrificial anode
Strategy.I.e. when corrosive medium reaches rich magnesium primary coat with aluminum or aluminum alloy substrate interface through coating, due to the corrosion potential of magnesium
Less than aluminium and the corrosion potential of aluminium alloy, with corrosive medium corrosion reaction occurs for magnesium first, so as to prevent that it is rotten that base metal from occurring
Erosion.
However, because magnesium powder is very active, would generally react rapidly the nonconducting corrosion of generation in application process
Product, substantial amounts of Mg corrosion product interrupt the electrical connection between active magnesium powder and base metal, and substrate aluminum or aluminum alloy will
Corrode, the cathodic protection effect failure of rich magnesium primary coat.By carrying out surface modification to magnesium powder, the reaction speed of magnesium powder is reduced
Degree, the cathodic protection life-span for extending rich magnesium primary coat is one of developing direction of rich magnesium priming paint.At present to the modification technology master of magnesium powder
Having advance carbon acid solution to carry out processing to magnesium powder makes one layer of magnesium carbonate of its Surface Creation.Although such a method improves rich magnesium and applied
The corrosion resisting property of layer, but the surface topography of magnesium powder is changed, and consume part magnesium powder.Surfactant-modified magnesium powder can be with
Magnesium powder is modified using surfactant and the chemisorbed on magnesium powder surface, organic carbochain on magnesium powder surface can reduce
The reaction speed of magnesium powder, so as to extend the service life of rich magnesium priming paint.
The content of the invention
Present invention aims at provide a kind of preparation method of magnesium stearate modification magnesium powder richness magnesium priming paint.
To achieve the above object, the technical solution adopted by the present invention is：
A kind of magnesium stearate is modified the preparation method of magnesium powder richness magnesium priming paint：
1) butyl acetate is mixed with magnesium stearate magnetic agitation, obtains mixed liquor a；Magnesium powder is added into mixed liquor a again,
24-48h is stirred at 20-40 DEG C, obtains the magnesium powder butyl acetate mixed liquor b of magnesium stearate modification, mixed liquor b is filtered, precipitation
Thing is dried at room temperature for, i.e., magnesium stearate is modified magnesium powder；
2) dimethylbenzene and n-butanol are added into epoxy resin (NPSN901 × 75), stirred, obtain mixed liquor c；Again
Polyimides (5115) is added in mixed liquor c, and stirred, obtains mixed liquor d；
Wherein, the mass ratio of epoxy resin and polyimides is 2-4:1；The mass ratio of dimethylbenzene and n-butanol is 1-2:1；
3) above-mentioned magnesium stearate modification magnesium powder is added in mixed liquor d, is uniformly mixing to obtain rich modified magnesium epoxy mixing
Liquid f, set aside for use, wherein, it is 0.63-0.83 that above-mentioned magnesium stearate, which is modified magnesium powder with mixed liquor d mass ratioes,：1.
The modified magnesium epoxy mixed liquor f produces epoxy richness magnesium coating sample coated on drying aluminium alloy substrate, drying at room temperature
Piece, wherein coat thickness are 100-200 μm.
The aluminium alloy substrate is that aluminium alloy substrate is polished, and is carried out clearly with distilled water and absolute ethyl alcohol respectively after polishing
Wash, the substrate bubble after cleaning is standby in absolute ethyl alcohol.
The aluminium alloy that the aluminium alloy substrate polishing is 50mm × 50mm, respectively with 140#, 400#, 600# and 800# sand
Paper is polished.
Preferably, magnesium powder is added into mixed liquor a the step 1), and 48h is stirred at 20 DEG C, obtains magnesium stearate modification
Magnesium powder butyl acetate mixed liquor b, mixed liquor b is filtered, sediment is dried at room temperature for 48h, i.e. magnesium stearate is modified magnesium powder.
Described preferred, the mass ratio of epoxy resin NPSN901 × 75 and polyimides 5115 is 3:1.
Described preferred, the mass ratio of toluene and n-butanol is 1:1.
Described preferred, modified magnesium powder and epoxy resin solution c mass ratio are 0.70:1.
The present invention has advantages below：
The preparation that magnesium stearate of the present invention is modified magnesium powder richness magnesium priming paint is by magnesium stearate polar end and magnesium powder surface pole
Property functional groups, magnesium powder surface formed one layer of organic monolayer.This monolayer will make the initial surface pattern of magnesium powder
Farthest retained.Also, the hydrophobicity of the organic company in surface will reduce corrosive medium and magnesium powder during corrosion protection
The formation of fine and close corrosion product in the reaction speed and corrosion process on surface, the use longevity extended during the corrosion protection of magnesium powder
Life.Rich magnesium coating prepared by the method will play significant role in corrosion-resistant fields such as aviation, ocean engineerings, be specially：
1. during being modified magnesium powder magnesium powder consumption does not occur for magnesium stearate, the utilization rate of magnesium powder will be improved, dropped as much as possible
Low use cost, accelerate the application process of rich magnesium priming paint.
2. magnesium stearate be modified magnesium powder be using magnesium stearate polar end and magnesium powder particle on polar functional group between
Chemical bonds magnesium powder surface formed one layer of very thin organic layer.This organic layer is very thin, and the primary morphology of magnesium powder can
Farthest to be retained.
3. magnesium stearate, which is modified the organic layer that magnesium powder surface is formed, has hydrophobic performance, corrosive medium and magnesium powder will be reduced
Contact, slow down the reaction speed of magnesium powder.Also, hydrophobic carbochain will reduce the formation of fine and close corrosion product, it is able to magnesium powder reaction
It is steady to carry out, and ensure contact of the corrosive medium with magnesium powder during corrosion protection, so as to add effective use of magnesium powder
Time, and effectively improve the service life of rich magnesium priming paint.
Brief description of the drawings
Fig. 1 is the infared spectrum that magnesium powder provided in an embodiment of the present invention and magnesium stearate are modified magnesium powder；
Fig. 2 is the SEM pictures of 500 times of the amplification of magnesium powder provided in an embodiment of the present invention and magnesium stearate modification magnesium powder；
Fig. 3 is the side SEM figures of rich modified 200 times of magnesium richness magnesium coating amplification after provided in an embodiment of the present invention soak 0 day
Piece；
Fig. 4 is the side SEM figures of rich modified 200 times of magnesium richness magnesium coating amplification after provided in an embodiment of the present invention soak 35 days
Piece.
Fig. 5 is the XRD test results of rich modified magnesium richness magnesium coating print after provided in an embodiment of the present invention soak 35 days.
Embodiment
Technical solution of the present invention is not limited to act embodiment set forth below, in addition between each embodiment
Any combination.
The present invention relates to rich magnesium priming paint, specifically a kind of magnesium stearate is modified the preparation method of magnesium powder richness magnesium priming paint.
The present invention is modified magnesium by the way that magnesium powder is dispersed in the butyl acetate solution of magnesium stearate and is stirred to obtain magnesium stearate
Powder, this is modified magnesium powder to prepare rich magnesium priming paint.The inventive method is not changing the situation of magnesium powder surface primary morphology and composition
Under can reduce magnesium powder reaction speed during cathodic protection, extend the service life of rich magnesium priming paint, will be in aviation, ocean
The corrosion-resistant fields such as engineering play significant role.
Embodiment 1
The preparation method of the magnesium-modified magnesium powder richness magnesium priming paint of hard acid follows the steps below：
First, magnesium stearate is modified the preparation of magnesium powder：100mL butyl acetate is added in 250mL conical flask first.Claim
70mg magnesium stearates are taken, and are added it in butyl acetate solution, magnetic agitation, obtain mixed liquor a.Weigh the magnesium powder of 400 mesh
8.0g, and add it in a, 24h is stirred at 20 DEG C, obtains the magnesium powder butyl acetate mixed liquor b of magnesium stearate modification.
2nd, the magnesium stearate for preparing step 1 is modified magnesium powder butyl acetate mixed liquor b and filtered, the magnesium powder after filtering
48h is dried at room temperature, i.e. magnesium stearate is modified magnesium powder.Magnesium powder and magnesium stearate are modified magnesium powder and characterized with infrared
(referring to Fig. 1).Modified magnesium powder is in 1465 and 1577cm-1The characteristic peak at place is that the stretching vibration of COO- functional groups in magnesium stearate is special
Levy peak, 2849 and 2916cm-1The characteristic peak at place is-CH2The characteristic absorption peak of-functional group.IR Characterization result illustrates magnesium powder table
Face is with the presence of magnesium stearate.Magnesium powder is with being modified the surface topography of magnesium powder referring to Fig. 2.Find out magnesium powder its rear table before modified from SEM figures
Face pattern does not change, illustrates that magnesium stearate is modified the primary morphology for remaining magnesium powder well.
3rd, the preparation of 2024 aluminium alloy substrates：2024 aluminium alloys are cut into 50mm × 50mm small pieces.Respectively with 140#,
400#, 600# and 800# sand paper are polished, and the substrate after polishing are cleaned with distilled water and absolute ethyl alcohol respectively, clearly
Substrate bubble after washing is standby in absolute ethyl alcohol.
4th, the epoxy resin of 3.0597 grams of NPSN901 × 75 is weighed with beaker.Weigh 1.3597 grams of dimethylbenzene and 1.3599 grams
N-butanol, it is well mixed, and is added in epoxy resin, stirs, obtain mixed liquor c.By 1.0198 gram of 5115 polyimides
It is added in mixed liquor c, and stirs, obtains mixed liquor d.
5th, 4.7594 grams of magnesium powders or modified magnesium powder are added in mixed liquor d, are uniformly mixing to obtain rich magnesium epoxy mixed liquor
E, set aside for use.Wherein, magnesium powder and the mass ratio that mixed liquor d is prepared in step 4 are 0.70:1.
6th, the aluminium alloy substrate for preparing step 3 dries up.Weigh 0.5048g mixed liquors e and be coated to aluminium alloy substrate
On, rich modified magnesium richness magnesium priming paint is produced after drying at room temperature 48h (referring to Fig. 3).As can be seen from the figure magnesium powder is mutual in rich magnesium coating
It is connected, the electrical connection during guarantee is anticorrosive, electrochemical cathode protection is provided for aluminium alloy base.
The thickness of dried rich magnesium coating is about 100 μm in step 6.
7th, rich magnesium coating prepared by step 6 is dipped into the NaCl solution that mass concentration is 3.5wt%, it is right after 35 days
The face cleaning of rich magnesium coating is detected, referring to Fig. 4.It can be seen that rich magnesium coating soak 35 days after its Cross Section Morphology not
Vary widely.Magnesium powder particle maintains primary morphology well in coating, and coating combined with aluminium substrate it is closer,
Illustrate that aluminium alloy base is not corroded.Fig. 5 is the XRD of print after soaking 35 days.There was only the feature of magnesium and substrate aluminium in figure
Peak, illustrates less in the magnesium powder consumption after immersion in 35 days in rich magnesium coating, and remaining to continue as aluminium substrate, to provide corrosion anti-
Shield acts on.
Embodiment 2
First, magnesium stearate is modified the preparation of magnesium powder：120mL butyl acetate is added in 250mL conical flask first.Claim
84mg magnesium stearates are taken, and are added it in butyl acetate solution, magnetic agitation, obtain mixed liquor a.Weigh the magnesium powder of 400 mesh
9.6g, and add it in a, 48h is stirred at 20 DEG C, obtains the magnesium powder butyl acetate mixed liquor b of magnesium stearate modification.
2nd, the magnesium stearate for preparing step 1 is modified magnesium powder butyl acetate mixed liquor b and filtered, the magnesium powder after filtering
48h is dried at room temperature, i.e. magnesium stearate is modified magnesium powder.
3rd, the preparation of 2024 aluminium alloy substrates：2024 aluminium alloys are cut into 50mm × 50mm small pieces.Respectively with 140#,
400#, 600# and 800# sand paper are polished, and the substrate after polishing are cleaned with distilled water and absolute ethyl alcohol respectively, clearly
Substrate bubble after washing is standby in absolute ethyl alcohol.
4th, the epoxy resin of 3.0597 grams of NPSN901 × 75 is weighed with beaker.Weigh 1.3597 grams of dimethylbenzene and 1.3599 grams
N-butanol, it is well mixed, and is added in epoxy resin, stirs, obtain mixed liquor c.By 1.0198 gram of 5115 polyimides
It is added in mixed liquor c, and stirs, obtains mixed liquor d.
5th, 4.7594 grams of magnesium powders or modified magnesium powder are added in mixed liquor d, are uniformly mixing to obtain rich magnesium epoxy mixed liquor
E, set aside for use.Wherein, magnesium powder and the mass ratio that mixed liquor d is prepared in step 4 are 0.70:1.
6th, the aluminium alloy substrate for preparing step 3 dries up.Weigh 0.5048g mixed liquors e and be coated to aluminium alloy substrate
On, rich modified magnesium richness magnesium priming paint is produced after drying at room temperature 48h.The thickness of dried rich magnesium coating is about 100 μm in step 6.
Embodiment 3
First, magnesium stearate is modified the preparation of magnesium powder：100mL butyl acetate is added in 250mL conical flask first.Claim
70mg magnesium stearates are taken, and are added it in butyl acetate solution, magnetic agitation, obtain mixed liquor a.Weigh the magnesium powder of 400 mesh
8.0g, and add it in a, 24h is stirred at 20 DEG C, obtains the magnesium powder butyl acetate mixed liquor b of magnesium stearate modification.
2nd, the magnesium stearate for preparing step 1 is modified magnesium powder butyl acetate mixed liquor b and filtered, the magnesium powder after filtering
48h is dried at room temperature, i.e. magnesium stearate is modified magnesium powder.
3rd, the preparation of 2024 aluminium alloy substrates：2024 aluminium alloys are cut into 50mm × 50mm small pieces.Respectively with 140#,
400#, 600# and 800# sand paper are polished, and the substrate after polishing are cleaned with distilled water and absolute ethyl alcohol respectively, clearly
Substrate bubble after washing is standby in absolute ethyl alcohol.
4th, the epoxy resin of 3.0597 grams of NPSN901 × 75 is weighed with beaker.Weigh 1.8130g dimethylbenzene and 0.9065g just
Butanol, it is well mixed, and is added in epoxy resin, stirs, obtain mixed liquor c.1.0198 gram of 5115 polyimides is added
Enter into mixed liquor c, and stir, obtain mixed liquor d.
5th, 4.7594 grams of magnesium powders or modified magnesium powder are added in mixed liquor d, are uniformly mixing to obtain rich magnesium epoxy mixed liquor
E, set aside for use.Wherein, magnesium powder and the mass ratio that mixed liquor d is prepared in step 4 are 0.70:1.
6th, the aluminium alloy substrate for preparing step 3 dries up.Weigh 0.5048g mixed liquors e and be coated to aluminium alloy substrate
On, rich modified magnesium richness magnesium priming paint is produced after drying at room temperature 48h.
The thickness of dried rich magnesium coating is about 100 μm in step 6.
Embodiment 4
First, magnesium stearate is modified the preparation of magnesium powder：100mL butyl acetate is added in 250mL conical flask first.Claim
70mg magnesium stearates are taken, and are added it in butyl acetate solution, magnetic agitation, obtain mixed liquor a.Weigh the magnesium powder of 400 mesh
8.0g, and add it in a, 24h is stirred at 20 DEG C, obtains the magnesium powder butyl acetate mixed liquor b of magnesium stearate modification.
2nd, the magnesium stearate for preparing step 1 is modified magnesium powder butyl acetate mixed liquor b and filtered, the magnesium powder after filtering
48h is dried at room temperature, i.e. magnesium stearate is modified magnesium powder.
3rd, the preparation of 2024 aluminium alloy substrates：2024 aluminium alloys are cut into 50mm × 50mm small pieces.Respectively with 140#,
400#, 600# and 800# sand paper are polished, and the substrate after polishing are cleaned with distilled water and absolute ethyl alcohol respectively, clearly
Substrate bubble after washing is standby in absolute ethyl alcohol.
4th, the epoxy resin of 3.0645 grams of NPSN901 × 75 is weighed with beaker.Weigh 1.5325g dimethylbenzene and 1.5322g just
Butanol, it is well mixed, and is added in epoxy resin, stirs, obtain mixed liquor c.1.5324 gram of 5115 polyimides is added
Enter into mixed liquor c, and stir, obtain mixed liquor d.
5th, 4.8268 grams of magnesium powders or modified magnesium powder are added in mixed liquor d, are uniformly mixing to obtain rich magnesium epoxy mixed liquor
E, set aside for use.Wherein, magnesium powder and the mass ratio that mixed liquor d is prepared in step 4 are 0.63:1.
6th, the aluminium alloy substrate for preparing step 3 dries up.Weigh 1.0165g mixed liquors e and be coated to aluminium alloy substrate
On, rich modified magnesium richness magnesium priming paint is produced after drying at room temperature 48h.
The thickness of dried rich magnesium coating is about 200 μm in step 6.
Embodiment 5
First, magnesium stearate is modified the preparation of magnesium powder：100mL butyl acetate is added in 250mL conical flask first.Claim
70mg magnesium stearates are taken, and are added it in butyl acetate solution, magnetic agitation, obtain mixed liquor a.Weigh the magnesium powder of 400 mesh
8.0g, and add it in a, 24h is stirred at 20 DEG C, obtains the magnesium powder butyl acetate mixed liquor b of magnesium stearate modification.
2nd, the magnesium stearate for preparing step 1 is modified magnesium powder butyl acetate mixed liquor b and filtered, the magnesium powder after filtering
48h is dried at room temperature, i.e. magnesium stearate is modified magnesium powder.
3rd, the preparation of 2024 aluminium alloy substrates：2024 aluminium alloys are cut into 50mm × 50mm small pieces.Respectively with 140#,
400#, 600# and 800# sand paper are polished, and the substrate after polishing are cleaned with distilled water and absolute ethyl alcohol respectively, clearly
Substrate bubble after washing is standby in absolute ethyl alcohol.
4th, the epoxy resin of 3.0534 grams of NPSN901 × 75 is weighed with beaker.Weigh 1.3569g dimethylbenzene and 1.3572g just
Butanol, it is well mixed, and is added in epoxy resin, stirs, obtain mixed liquor c.1.0178 gram of 5115 polyimides is added
Enter into mixed liquor c, and stir, obtain mixed liquor d.
5th, 5.6318 grams of magnesium powders or modified magnesium powder are added in mixed liquor d, are uniformly mixing to obtain rich magnesium epoxy mixed liquor
E, set aside for use.Wherein, magnesium powder and the mass ratio that mixed liquor d is prepared in step 4 are 0.83:1.
6th, the aluminium alloy substrate for preparing step 3 dries up.Weigh 0.4989g mixed liquors e and be coated to aluminium alloy substrate
On, rich modified magnesium richness magnesium priming paint is produced after drying at room temperature 48h.
The thickness of dried rich magnesium coating is about 100 μm in step 6.
Claims (4)
1. a kind of magnesium stearate is modified the preparation method of magnesium powder richness magnesium priming paint, it is characterised in that：
1）Butyl acetate is mixed with magnesium stearate magnetic agitation, obtains mixed liquor a；Magnesium powder is added into mixed liquor a again, 20 DEG C
Lower stirring 48h, the magnesium powder butyl acetate mixed liquor b of magnesium stearate modification is obtained, mixed liquor b is filtered, precipitation is done at room temperature
Dry 48h, i.e. magnesium stearate are modified magnesium powder；
2）Dimethylbenzene and n-butanol are added into epoxy resin NPSN901 × 75, stirred, obtains mixed liquor c；Again by polyamides
Imines is added in mixed liquor c, and is stirred, and obtains mixed liquor d；
Wherein, the mass ratio of epoxy resin and polyimides is 2-4:1；The mass ratio of dimethylbenzene and n-butanol is 1-2:1；
3）Above-mentioned magnesium stearate modification magnesium powder is added in mixed liquor d, is uniformly mixing to obtain rich magnesium epoxy mixed liquor f, is stood
It is stand-by, wherein, it is 0.63-0.83 that above-mentioned magnesium stearate, which is modified magnesium powder with mixed liquor d mass ratioes,：1.
2. the magnesium stearate as described in claim 1 is modified the preparation method of magnesium powder richness magnesium priming paint, it is characterised in that：The rich magnesium
Epoxy mixed liquor f produces epoxy richness magnesium coating print coated on drying aluminium alloy substrate, drying at room temperature, and wherein coat thickness is
100-200μm。
3. the magnesium stearate as described in claim 2 is modified the preparation method of magnesium powder richness magnesium priming paint, it is characterised in that：The aluminium closes
Auri piece is that aluminium alloy substrate is polished, and is cleaned respectively with distilled water and absolute ethyl alcohol after polishing, the substrate bubble after cleaning
It is standby in absolute ethyl alcohol.
4. the magnesium stearate as described in claim 3 is modified the preparation method of magnesium powder richness magnesium priming paint, it is characterised in that：The aluminium closes
The polishing of auri piece is 50 mm × 50mm aluminium alloy, is polished respectively with 140#, 400#, 600# and 800# sand paper.
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| CN201510617105.6A CN105131790B (en) | 2015-09-24 | 2015-09-24 | Magnesium stearate is modified the preparation method of magnesium powder richness magnesium priming paint |
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| CN201510617105.6A CN105131790B (en) | 2015-09-24 | 2015-09-24 | Magnesium stearate is modified the preparation method of magnesium powder richness magnesium priming paint |
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| CN105131790B true CN105131790B (en) | 2017-12-26 |
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| CN110396350B (en) * | 2019-07-29 | 2021-12-24 | 广东好邦石墨烯新材料科技有限公司 | Anticorrosive paint and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1878619A (en) * | 2003-11-13 | 2006-12-13 | Ndsu研究基金会 | Magnesium rich coatings and coating systems |
| CN103571305A (en) * | 2013-10-25 | 2014-02-12 | 中山大桥化工集团有限公司 | Epoxy-magnesium-rich coating and preparation method thereof |
-
2015
- 2015-09-24 CN CN201510617105.6A patent/CN105131790B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1878619A (en) * | 2003-11-13 | 2006-12-13 | Ndsu研究基金会 | Magnesium rich coatings and coating systems |
| CN103571305A (en) * | 2013-10-25 | 2014-02-12 | 中山大桥化工集团有限公司 | Epoxy-magnesium-rich coating and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 铝合金保护用富镁底漆的研制及其性能研究;戈成岳 等;《涂料工业》;20130430;第43卷(第4期);全文 * |
| 镁粉表面改性的初步研究;李宝芳;《机械管理开发》;20060228(第1期);第1页的引言、第2页的第3节 * |
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