CN102181231A - Preparation method of water-based environmentally-friendly anticorrosion paint - Google Patents
Preparation method of water-based environmentally-friendly anticorrosion paint Download PDFInfo
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Abstract
The invention relates to a preparation method of an anticorrosion paint, in particular to a preparation method of a water-based environmentally-friendly anticorrosion paint, which is mainly used for solving the technical problems that the product performance cannot be brought into full play, the comprehensive product performance cannot be reflected to the maximum extent due to the selecting and the matching of a raw material structure and the performance price ratio and the like. The method comprises the following steps of: adding water into a dispersion machine, starting the dispersion machine at a low speed and adding a dispersant, a flash rust agent, a multifunctional aid, a defoaming agent and a preservative for performing low-speed dispersing; adding a composite phosphate ferrotitanium inhibitive pigment, zinc phosphate, iron red, calcite and sericite for performing low-speed dispersing; switching to a medium-speed gear, adding a defoaming agent, silica sol, alcohol ester-12, an anti-freezing agent and a flatting agent for performing high-speed dispersing; and adding an emulsion, dispersing, adding a pH value regulating agent for adjusting the pH value, slowly adding a thickening agent and an inhibitor, verifying viscosity, filtering and canning to obtain a finished product.
Description
Technical field
The present invention relates to a kind of preparation method of rust-inhibiting paint, especially relate to a kind of preparation method of aqueous, environmental protective rust-inhibiting paint.
Background technology
Along with the raising of development and national economy and living standards of the people, the application of paints scope constantly enlarges, and the strictness day by day of the enhancing of people's environmental consciousness and environmental regulation is more and more higher to the requirement of coating.The environmental regulation of world's Sustainable development is constantly strengthened, and impels coatings industry to develop this big trend to eco-friendly direction and can not change.
According to data, in countries such as the U.S., Japan, Canada, the direct economic loss that corrosion causes accounts for the 1%-4% of total value of production in national economy, and the iron and steel of annual rust corrosion accounts for 20% of annual production.Antirust, anti-corrosive occupies crucial status.China is big steel country, and iron and steel and steel product must the processing of strict process antirust, anti-corrosive could guarantee its work-ing life, statistics, the financial loss that causes in the annual metallic corrosion of China accounts for 4% of gross national product, so rust-proof antiseptic paint has a large capacity and a wide range in China's coating products.Rust-proof antiseptic paint has become the focus that industry is paid close attention to over past ten years, is subjected to the latency of market demand to influence the steel demand and presents a rapidly rising trend, and this is the prime mover that increases fast of the whole coating industry of China just.For a long time, Coating Industry in Our Country is grabbed the series product that all kinds of antirust, anti-corrosive types are developed in continuous exploratory development always as an important action, and through the arduous effort of decades, the rust-proof antiseptic paint product of China has had tremendous development.In the production and construction process of the solvent-borne type protective system of widespread use at present, a large amount of organic solvents evaporate in the atmosphere, serious environment pollution and harm humans health.Therefore, the development of China's anti-corrosive antirusting paint is faced with stern challenge, seeking new technology outlet is the needs of the times, following coating development trend develops towards high-performance, energy-saving and environmental protection, solvent-free direction and multifunction direction, various eco-friendly coating obtain the approval in market, and the Water-borne modification of coating is considered to the final developing direction of coating.
This disclosure of the Invention of the watersoluble metal self-drying antirusting paint that Chongqing Snaibo Dope Co., Ltd. develops [Chinese patent: CN101429402 open (bulletin) day): 2009.05.13] a kind of watersoluble metal self-drying antirusting paint, it is characterized in that by following components in part by weight mixed must: SD-688 pure-acrylic emulsion 15-25 part, SD-588 benzene emulsion 15-25 part, SE-60 epoxy emulsion 15-25 part, urethane resin 10-15 part, nano-organosilicon emulsion 2-5 part, film coalescence aid 10-20 part, nano level rust-stabilising pigment 5-10 part, water-based siccative 1-5 part, water-based anti-sedimentation agent 5-10 part, water-based extender 2-5 part, aqueous diluent 2-20 part.The present invention selects for use by improving film forming matter---pure-acrylic emulsion, benzene emulsion, epoxy, urethane and organosilicon, and add various auxiliary agents, and the temperature of film forming matter is reduced, increase solids content simultaneously, and allow thinner volatilize rapidly, to reach fast filming, antiseptic and rustproof purpose.
The said products has certain effect as the representative of the comparatively matured product of waterborne anti-rust lacquer on product performance; Simultaneously also have certain deficiency, the product environmental protection concept has reached certain height, but product performance fail fundamentally to obtain considerable performance, and because of the selection collocation of raw material mix, cost performance can not embody the product over-all properties to greatest extent.
Summary of the invention
The present invention provides a kind of preparation method of aqueous, environmental protective rust-inhibiting paint, it mainly is to solve the product existing in prior technology performance to fail fundamentally to obtain considerable performance, because of the selection of raw material mix collocation, cost performance can not embody the technical problem of product over-all properties etc. to greatest extent.
Above-mentioned technical problem of the present invention is mainly solved by following technical proposals:
The preparation method of a kind of aqueous, environmental protective rust-inhibiting paint of the present invention is characterized in that described method is:
A. the water that in dispersion machine, adds the 15-20 weight part, low speed is opened dispersion machine, the dispersion of adding 0.5-1.0 weight part, the agent of sudden strain of a muscle rust, the multifunctional assistant of 0.1-0.5 weight part, the defoamer of 0.1-0.5 weight part, the sanitas of 0.1-0.5 weight part disperse thereby carry out low speed;
B. add the composite phosphate ferrotitanium rust-stabilising pigment of 3-5 weight part, the zinc phosphate of 1-5 weight part, the iron oxide red of 5-10 weight part, the calcite of 20-25 weight part, the sericite of 3-5 weight part, carry out high speed dispersion;
C. behind the gear level, add the defoamer of 0.1-0.5 weight part, the silicon sol of 5-8 weight part, the alcohol ester-12 of 5-10 weight part, the frostproofer of 1-2 weight part, the flow agent of 0.1-0.5 weight part, carry out high speed dispersion then;
D. disperse after adding the emulsion of 30-40 weight part, the pH value conditioning agent that adds the 0.1-0.2 weight part is again regulated pH value=8-9, slowly add the thickening material of 0.3-1.0 weight part, the inhibiter of 0.1-0.5 weight part, after check viscosity is qualified, filter the canned finished product that promptly goes out.
The present invention adopts the inorganic compounding rust-stabilising pigment to substitute traditional plumbous based material in the middle of this project in research and makes obtain same effect on performance, its rust-proof mechanism: phosphate radical and steel surface atomic reaction generate the tertiary iron phosphate complex salt, the tertiary iron phosphate complex salt forms protective layer attached to steel surface securely, have durable protective and reasonableness, product more meets environmental protection concept, and this is the spotlight that the present invention uses novel material; Sum up to draw by repetition test and have a large amount of emulsifying agents suctions in the common benzene emulsion sintetics, the acrylic acid modified emulsion of soap-free polymerization of utilization has effectively been controlled the amount (more being to react away post-synthesis phase) of emulsifying agent in post-synthesis phase, good a lot of than traditional emulsion of its salt water resistance performance, the construction effect and the compactness of filming can effectively hinder the erosion to iron and steel such as air; Phosphoric acid salt dispersion agent itself is applied in this development and Design as resistance rust material, the dispersant system that organic polyacrylate and poly-phosphate combine is collaborative to be disperseed, make that dispersive ability and package stability are better, because in the majorityly in the conventional latex system using with the single type dispersion agent, polyacrylate uses in the majority.It is bigger to use polyacrylic acid dipersant dispersion efficiency influenced by molecular weight separately, its molecular weight is big more, package stability is good more, the polyacrylate polar phase is to less, the electric density that the coverage pigment surface is produced is little, plays shock absorption attached to particle surface, forms sterically hindered between particle, but its specific molecule structure makes it produce the bridging effect again easily between single granules of pigments, therefore still might form reunion.Opposite poly-phosphate has the strong characteristics of polarity, the rapid coverage pigment particle surface of energy in dispersion system, produce high charge density, play stabilization, be used the bridging that can prevent between single granules of pigments, electrostatic stabilization and locus synergy can make whole dispersion system have good dispersiveness and package stability.
Because the big inherent characteristics of steam heat-transmission, aqueous, environmental protective rust-inhibiting paint relatively dry is slow, easy sagging, and there is certain degree of difficulty in disposable one-tenth thick film, and application property also is a big difficult point of water-miscible paint.These research and development system this to this singularity, use thixotroping auxiliary agent thickened systems to change the rheological of coating, find progressively after the use that aspects such as coating application thixotropy, levelling reach ideal effect.Filler also is the vital tissue part of coating products, and paint film is had enhancement, improves the hardness of filming, and application property also can reduce the residualinternal stress in the dried coating film process simultaneously, improves the sticking power of filming thereby help.Anything all has two-sidedness, can obviously change a series of as mechanical strength, heat-resisting reinforcement in, the excessive compactness that also affects paint film of dosage, finally, directly influence the resistance to salt water of paint film, the present invention has taken into full account its stake, and addition is also as the high spot reviews object in the test in later stage.
The present invention selects raw-material characteristics for use:
Resistance to salt water: filmogen, rust-stabilising pigment, amount of filler is bigger to the resistance to salt water influence; The influence of each level of factor is A3B3C1 in proper order.Emulsion, rust-stabilising pigment, amount of filler has consistence to the influence of resistance to salt water.Difference is emulsion kind difference, and the water tolerance difference clearly.Under the same level, the A1 paint film foaming that eases back earlier behind the saline soak, it is turbid to become rusty again, only 12 days; And A2, A3 have only rust turbid to beginning to whole, not foaming, and this point proves absolutely that the compactness of paint film is most important; wet sticking power is also very important, if only self densification of paint film, and wet sticking power would be generally not good; then force of cohesion is excessive, and paint film also may be peeled off from whole basal plane, loses protection.Reason is resolved: ordinary emulsion building-up process emulsifying agent is last exists in the water tolerance that influence paint film, because of emulsifying agent hydrophilic, long period of soaking, the high molecular emulsion particle absorbs water influences sticking power under water; And the self-crossing emulsion film forming is fine and close relatively, the hydrophobic relatively paint film densification of soap-free polymerization emulsion paint film, and sticking power is influenced relatively not obvious under water, so even become rusty turbid also non-foaming.More different dispersion agents influence situation to the dispersion effect, water-resistance property of coating etc. of color stuffing system in the prescription, and phosphoric acid salt dispersion agent dispersion effect one is good, but unstable, and the phosphate radical of generation can produce passivation with the iron and steel reaction; The polyacrylic acid sodium salt dispersion effect is general but stability is good, and the excessive paint film that easily makes of the ion of receiving causes rust.Filler has enhancement to paint film, and the excessive compactness that also affects paint film of dosage is final, directly influences the resistance to salt water of paint film;
Sticking power: the influence of (binding agent) emulsion has consistence, and it has bigger contribution to sticking power; The adding of amount of filler is to coating adhesion (drawing circle) level, remarkably influenced is arranged, along with the increase of amount of filler, coating adhesion progression rises earlier and afterwards descends, and analyzes the reason filler and improves the hardness of filming, application property, also reduce the residualinternal stress in the dried coating film process simultaneously, improve the sticking power film, but dosage paint film resin-pigment ratio when a certain amount of descends rapidly thereby help, influence cohesive strength, final sticking power descends rapidly.In conjunction with indexs such as resistance to salt waters, analysis-by-synthesis adds the 250g filler to salt water resistance in the benchmark prescription, and influence such as sticking power relaxes relatively.
Stability: poly-phosphate has strong polarity, and the coverage pigment particle surface produces high charge density rapidly, plays electrostatic stabilization.The polyacrylate polar phase is to less, and the electric density that the coverage pigment surface is produced is few, but it plays shock absorption attached to particle surface, forms sterically hinderedly between particle, plays the effect of steric stabilization.But the molecular structure of polyacrylate makes it produce the bridging effect easily between single granules of pigments.Therefore, only use the polyacrylic acid dipersant in the system, still might form reunion.When polyacrylate and poly-phosphate dispersion agent were used, the high charge density that strong polar poly-phosphate forms on the granules of pigments surface was to prevent the bridging between the single granules of pigments.At this moment, electrostatic stabilization and steric stabilization act synergistically and make coating have good dispersiveness and package stability simultaneously.Select poly-phosphate and polyacrylic acid dipersant to be used, dispersant dosage is 0.2% poly-phosphate, ten 0.35% polyacrylates, and adopts the poly-phosphate dispersion agent of medium chain (n=6-10); Though the polyacrylic acid dipersant is an ionic, it increases little to system's polarity, and the molecular weight of polyacrylic acid dipersant is selected 3000-5000's.When polyacrylic acid dipersant and poly-phosphate dispersion agent were used, dispersive ability and package stability were best.
As preferably, described step b high speed is sent into raw material sand mill again and is carried out sand milling after disperseing, and makes behind the sand milling material fineness be≤45um.
As preferably, low speed dispersive speed is≤400r/min among the described step a.
As preferably, low speed dispersive speed is 200r/min among the described step a, after the dispersion again middling speed stirred 5-10 minute, wherein the speed that stirs of middling speed is 400-600r/min.
As preferably, described step b high speed dispersive speed is 450-650r/min.
As preferably, the middling speed dispersive speed among the described step c is 400-600r/min.
As preferably, the described step c high speed dispersive time is 5-10 minutes, and the dispersive time is 10 minutes in the steps d.
As preferably, the rust agent that disperses among the described step a, looses is NC, SN-5040, and multifunctional assistant is AMP-95, and defoamer is 208, and sanitas is CL-15.
As preferably, defoamer is NXZ among the described step c, and flow agent is UH420.
As preferably, the pH value conditioning agent is ammoniacal liquor or AMP-95 in the described steps d, and thickening material is D-108, and inhibiter is SER-ADFAl79.
Therefore; the present invention has substituted traditional plumbous based material and has made obtain same effect on performance; its phosphate radical and steel surface atomic reaction generate the tertiary iron phosphate complex salt; the tertiary iron phosphate complex salt forms protective layer attached to steel surface securely; have durable protective and reasonableness, product more meets environmental protection concept.
Embodiment
Below by embodiment, technical scheme of the present invention is described in further detail.
Embodiment 1: the preparation method of a kind of aqueous, environmental protective rust-inhibiting paint of this example, and its method is:
A. the water that in dispersion machine, adds 15 weight parts, low speed is opened dispersion machine, add the sanitas CL-15 of defoamer 208,0.1 weight part of AMP-95,0.1 weight part of SN-5040,0.1 weight part of NC, 0.2 weight part of 0.3 weight part, disperseed 5 minutes thereby carry out low speed;
B. add the composite phosphate ferrotitanium rust-stabilising pigment of 3 weight parts, the zinc phosphate of 1 weight part, the iron oxide red of 5 weight parts, 800 order calcites of 20 weight parts, 1250 order sericites of 3 weight parts, carried out high speed dispersion 30 minutes, the water that adds 60 weight parts is put into sand mill and is carried out sand milling, makes behind the sand milling material fineness be≤45um;
C. behind the gear level, add the defoamer NXZ of 0.1 weight part, the silicon sol of 5 weight parts, the alcohol ester-12 of 5 weight parts, the frostproofer of 1 weight part, the flow agent UH420 of 0.1 weight part, carried out high speed dispersion then 10 minutes;
D. disperse after adding the emulsion of 30 weight parts, the AMP-95 that adds 0.1 weight part again regulates pH value=8-9, slowly adds the thickening material D-108 of 0.3 weight part, the inhibiter SER-ADFA179 of 0.1 weight part, check viscosity qualified after, filter the canned finished product that promptly goes out.
Embodiment 2: the preparation method of a kind of aqueous, environmental protective rust-inhibiting paint of this example, and its method is:
A. the water that in dispersion machine, adds 18 weight parts, low speed is opened dispersion machine, add the sanitas CL-15 of defoamer 208,0.3 weight part of AMP-95,0.3 weight part of SN-5040,0.3 weight part of NC, 0.4 weight part of 0.4 weight part, disperseed 5 minutes thereby carry out low speed;
B. add the composite phosphate ferrotitanium rust-stabilising pigment of 4 weight parts, the zinc phosphate of 3 weight parts, the iron oxide red of 8 weight parts, 800 order calcites of 22 weight parts, 1250 order sericites of 4 weight parts, carried out high speed dispersion 30 minutes, the water that adds 60 weight parts is put into sand mill and is carried out sand milling, makes behind the sand milling material fineness be≤45um;
C. behind the gear level, add the defoamer NXZ of 0.3 weight part, the silicon sol of 7 weight parts, the alcohol ester-12 of 8 weight parts, the frostproofer of 1.5 weight parts, the flow agent UH420 of 0.3 weight part, carried out high speed dispersion then 10 minutes;
D. disperse after adding the emulsion of 35 weight parts, the ammoniacal liquor that adds 0.15 weight part is again regulated pH value=8-9, slowly adds the thickening material D-108 of 0.5 weight part, the inhibiter SER-ADFA179 of 0.4 weight part, check viscosity qualified after, filter the canned finished product that promptly goes out.
Embodiment 3: the preparation method of a kind of aqueous, environmental protective rust-inhibiting paint of this example, and its method is:
A. the water that in dispersion machine, adds 20 weight parts, low speed is opened dispersion machine, add the sanitas CL-15 of defoamer 208,0.5 weight part of AMP-95,0.5 weight part of SN-5040,0.3 weight part of NC, 0.5 weight part of 1.0 weight parts, disperseed 5 minutes thereby carry out low speed;
B. add the composite phosphate ferrotitanium rust-stabilising pigment of 5 weight parts, the zinc phosphate of 5 weight parts, the iron oxide red of 10 weight parts, 800 order calcites of 25 weight parts, 1250 order sericites of 5 weight parts, carried out high speed dispersion 30 minutes, the water that adds 60 weight parts is put into sand mill and is carried out sand milling, makes behind the sand milling material fineness be≤45um;
C. behind the gear level, add the defoamer NXZ of 0.5 weight part, the silicon sol of 8 weight parts, the alcohol ester-12 of 10 weight parts, the frostproofer of 2 weight parts, the flow agent UH420 of 0.5 weight part, carried out high speed dispersion then 10 minutes;
D. disperse after adding the emulsion of 40 weight parts, the AMP-95 that adds 0.2 weight part again regulates pH value=8-9, slowly adds the thickening material D-108 of 1.0 weight parts, the inhibiter SER-ADFA179 of 0.5 weight part, check viscosity qualified after, filter the canned finished product that promptly goes out.
The above only is specific embodiments of the invention, but constitutional features of the present invention is not limited thereto, and any those skilled in the art is in the field of the invention, and the variation of being done or modify all is encompassed among the claim of the present invention.
Claims (10)
1. the preparation method of an aqueous, environmental protective rust-inhibiting paint is characterized in that described method is:
A. the water that in dispersion machine, adds the 15-20 weight part, low speed is opened dispersion machine, the dispersion of adding 0.5-1.0 weight part, the agent of sudden strain of a muscle rust, the multifunctional assistant of 0.1-0.5 weight part, the defoamer of 0.1-0.5 weight part, the sanitas of 0.1-0.5 weight part disperse thereby carry out low speed;
B. add the composite phosphate ferrotitanium rust-stabilising pigment of 3-5 weight part, the zinc phosphate of 1-5 weight part, the iron oxide red of 5-10 weight part, the calcite of 20-25 weight part, the sericite of 3-5 weight part, carry out high speed dispersion;
C. behind the gear level, add the defoamer of 0.1-0.5 weight part, the silicon sol of 5-8 weight part, the alcohol ester-12 of 5-10 weight part, the frostproofer of 1-2 weight part, the flow agent of 0.1-0.5 weight part, carry out high speed dispersion then;
D. disperse after adding the emulsion of 30-40 weight part, the pH value conditioning agent that adds the 0.1-0.2 weight part is again regulated pH value=8-9, slowly add the thickening material of 0.3-1.0 weight part, the inhibiter of 0.1-0.5 weight part, after check viscosity is qualified, filter the canned finished product that promptly goes out.
2. the preparation method of a kind of aqueous, environmental protective rust-inhibiting paint according to claim 1, it is characterized in that described step b high speed is disperseed after, again raw material is sent into sand mill and is carried out sand milling, make behind the sand milling material fineness be≤45um.
3. the preparation method of a kind of aqueous, environmental protective rust-inhibiting paint according to claim 1 is characterized in that low speed dispersive speed is≤400r/min among the described step a.
4. the preparation method of a kind of aqueous, environmental protective rust-inhibiting paint according to claim 1 is characterized in that low speed dispersive speed is 200r/min among the described step a, after the dispersion again middling speed stirred 5-10 minute, wherein the speed that stirs of middling speed is 400-600r/min.
5. the preparation method of a kind of aqueous, environmental protective rust-inhibiting paint according to claim 1 is characterized in that described step b high speed dispersive speed is 450-650r/min.
6. the preparation method of a kind of aqueous, environmental protective rust-inhibiting paint according to claim 1 is characterized in that the middling speed dispersive speed among the described step c is 400-600r/min.
7. the preparation method of a kind of aqueous, environmental protective rust-inhibiting paint according to claim 1 is characterized in that the described step c high speed dispersive time is 5-10 minute, and the dispersive time is 10 minutes in the steps d.
8. the preparation method of a kind of aqueous, environmental protective rust-inhibiting paint according to claim 1, the rust agent that it is characterized in that disperseing among the described step a, looses is NC, SN-5040, and multifunctional assistant is AMP-95, and defoamer is 208, and sanitas is CL-15.
9. the preparation method of a kind of aqueous, environmental protective rust-inhibiting paint according to claim 1 is characterized in that defoamer is NXZ among the described step c, and flow agent is UH420.
10. the preparation method of a kind of aqueous, environmental protective rust-inhibiting paint according to claim 1 is characterized in that the pH value conditioning agent is ammoniacal liquor or AMP-95 in the described steps d, and thickening material is D-108, and inhibiter is SER-ADFAl79.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102746766A (en) * | 2012-07-23 | 2012-10-24 | 江苏华夏制漆科技有限公司 | Water -borne anticorrosion paint and method for preparing same |
| CN103509417A (en) * | 2013-03-22 | 2014-01-15 | 江门市坚坝涂料科技有限公司 | Water-based anti-rust paint and manufacturing technique thereof |
| CN104927521A (en) * | 2015-06-10 | 2015-09-23 | 柳州弘天科技有限公司 | Antirust paint |
| CN105885645A (en) * | 2016-01-27 | 2016-08-24 | 浙江传化涂料有限公司 | Preparation method of waterborne rusty epoxy coating |
| CN106752957A (en) * | 2016-12-01 | 2017-05-31 | 河池市技术开发中心 | For the antirust primer base of mining machinery |
| CN108192443A (en) * | 2018-01-24 | 2018-06-22 | 合肥尚强电气科技有限公司 | Antirust paint for power equipment |
| CN116218310A (en) * | 2023-04-07 | 2023-06-06 | 青岛科技大学 | Silica sol modified acrylic acid anticorrosive paint and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102746766A (en) * | 2012-07-23 | 2012-10-24 | 江苏华夏制漆科技有限公司 | Water -borne anticorrosion paint and method for preparing same |
| CN102746766B (en) * | 2012-07-23 | 2014-11-26 | 江苏华夏制漆科技有限公司 | Water-borne anticorrosion paint and method for preparing same |
| CN103509417A (en) * | 2013-03-22 | 2014-01-15 | 江门市坚坝涂料科技有限公司 | Water-based anti-rust paint and manufacturing technique thereof |
| CN104927521A (en) * | 2015-06-10 | 2015-09-23 | 柳州弘天科技有限公司 | Antirust paint |
| CN105885645A (en) * | 2016-01-27 | 2016-08-24 | 浙江传化涂料有限公司 | Preparation method of waterborne rusty epoxy coating |
| CN105885645B (en) * | 2016-01-27 | 2020-04-24 | 浙江传化涂料有限公司 | Preparation method of water-based rusty epoxy coating |
| CN106752957A (en) * | 2016-12-01 | 2017-05-31 | 河池市技术开发中心 | For the antirust primer base of mining machinery |
| CN108192443A (en) * | 2018-01-24 | 2018-06-22 | 合肥尚强电气科技有限公司 | Antirust paint for power equipment |
| CN116218310A (en) * | 2023-04-07 | 2023-06-06 | 青岛科技大学 | Silica sol modified acrylic acid anticorrosive paint and preparation method thereof |
| CN116218310B (en) * | 2023-04-07 | 2024-05-28 | 青岛科技大学 | Silica sol modified acrylic acid anticorrosive paint and preparation method thereof |
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