CN109705696A - A kind of nano-silicon dioxide modified epoxy coating - Google Patents
A kind of nano-silicon dioxide modified epoxy coating Download PDFInfo
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Abstract
The invention discloses a kind of nano-silicon dioxide modified epoxy coating, raw material includes: that 55-70 parts of epoxy resin, 8-15 parts of chlorinated rubber, 5-18 parts of silicone resin, 9-15 parts of alkyd resin, 1-3 parts of graphene oxide, 3-8 parts of nano silica, 2-8 parts of charcoal powder, 1-3 parts of silicon carbide, nano-titanium be 0.3-1.8 parts black, 2-6 parts of precipitation method barium sulfate, 0.7-3 parts of bamboo fibre, 3-9 parts of basalt scale, 2-8 parts of nano aluminium oxide, 9-25 parts of curing agent, 0.1-1 parts of 1- pyrene butyric acid, 20-30 parts of solvent, 0.2-1.5 parts of auxiliary agent by weight;The curing agent be trimellitic anhydride N-butyl, 2-ethyl-4-methylimidazole, zinc acrylate resin, boron amine curing agent 594 mixture.Nano-silicon dioxide modified epoxy coating proposed by the present invention, intensity is high, and heat resistance and wearability are good, excellent anti-corrosion performance.
Description
Technical field
The present invention relates to technical field of coatings more particularly to a kind of nano-silicon dioxide modified epoxy coatings.
Background technique
Epoxy resin is one of most common thermosetting resin, with excellent caking property, anticorrosive property, and intensity
Height, epoxy coating made of it have been widely used for automobile, shipbuilding, aviation, machinery, chemical industry and large-scale water conservancy at present
Engineering and civil construction industry etc.;However, the poor heat resistance of epoxy resin, wearability is not very well, to apply made of it
Material haves the defects that heat-resistance of film wearability is undesirable, limits its application.
Summary of the invention
Technical problems based on background technology, the invention proposes a kind of nano-silicon dioxide modified epoxy resin to apply
Material, intensity is high, and heat resistance and wearability are good, excellent anti-corrosion performance.
A kind of nano-silicon dioxide modified epoxy coating proposed by the present invention, raw material includes: epoxy by weight
55-70 parts of resin, 8-15 parts of chlorinated rubber, 5-18 parts of silicone resin, 9-15 parts of alkyd resin, 1-3 parts of graphene oxide, nanometer
3-8 parts of silica, 2-8 parts of charcoal powder, 1-3 parts of silicon carbide, nano-titanium be 0.3-1.8 parts black, 2-6 parts of precipitation method barium sulfate, bamboo
0.7-3 parts of fiber, 3-9 parts of basalt scale, 2-8 parts of nano aluminium oxide, 9-25 parts of curing agent, 0.1-1 parts of 1- pyrene butyric acid, solvent
20-30 parts, 0.2-1.5 parts of auxiliary agent;
Wherein, the curing agent is trimellitic anhydride N-butyl, 2-ethyl-4-methylimidazole, zinc acrylate resin, boron amide class are consolidated
The mixture of agent 594.
Preferably, the nano silica is modified manometer silicon dioxide;The modified manometer silicon dioxide according to
Prepared by lower technique: cetyl trimethylammonium bromide, sodium metasilicate, rare earth compound being mixed with distilled water, adjusted after stirring
Section pH value is 8-9, stirs 8-11h at normal temperature, and calcining obtains material A after standing, be filtered, washed, drying;With silane coupling agent
KH-550 is that modifying agent is modified material A, obtains material B;Material B, the formalin that mass fraction is 37% are mixed,
5-7.5h is reacted in ice-water bath, the toluene solution of parahydroxyben-zaldehyde is then added, 4-6h is reacted at 60-75 DEG C, is reacted
After wash, be dried to obtain the modified manometer silicon dioxide.
Preferably, cetyl trimethylammonium bromide, sodium metasilicate, dilute in the preparation process of modified manometer silicon dioxide
The weight ratio of earth compounds is 0.3-0.5:2-3:0.03-0.08;Silane resin acceptor kh-550, material A weight ratio be 0.4-
0.7:1;The weight ratio of formalin, parahydroxyben-zaldehyde that material B, mass fraction are 37% is 1.4-1.8:0.4-0.7:
1.5-2.5。
Preferably, in the preparation process of modified manometer silicon dioxide, the temperature of calcining is 490-520 DEG C, time 3-
5h。
Preferably, in the preparation process of modified manometer silicon dioxide, the rare earth compound be holmium nitrate, erbium nitrate,
The mixture of one or more of samaric nitrate, yttrium nitrate.
Preferably, the graphene oxide is the graphene oxide of p-phenylenediamine functionalization.
Preferably, the basalt scale is polyaniline-modified basalt scale.
Preferably, the average grain diameter of the nano aluminium oxide is 30-85nm.
Preferably, in curing agent, trimellitic anhydride N-butyl, 2-ethyl-4-methylimidazole, zinc acrylate resin, boron amide class are solid
The weight ratio of agent 594 is 2-5:0.1-1.2:0.5-2:1-1.7.
Preferably, the auxiliary agent includes anti-settling agent, wetting dispersing agent, defoaming agent and levelling agent, and anti-settling agent, wetting and dispersing
The weight ratio of agent, defoaming agent and levelling agent is 2.3-3.4:0.3-0.8:0.1-0.7:0.1-1.
Nano-silicon dioxide modified epoxy coating of the present invention can be prepared according to conventional epoxy coating
Each raw material is uniformly mixed and forms by technique.
Nano-silicon dioxide modified epoxy coating of the present invention, using epoxy resin as major ingredient in raw material, simultaneously
Be added to chlorinated rubber, silicone resin, alkyd resin and its cooperate, chlorinated rubber therein has the corrosive mediums such as water vapour
Barrier property, silicone resin heat-resisting quantity is good, after chlorinated rubber, silicone resin and epoxy resin and alkyd resin cooperation, plays each
The advantages of raw material, improves the safeguard function of film, assigns coating excellent corrosion resistance, while heat resistance and flexibility are good;
Graphene oxide, nano silica, charcoal powder, silicon carbide, nano-titanium be black, precipitation method barium sulfate, bamboo fibre, basalt squama
Piece, nano aluminium oxide cooperation improve the intensity of coating as in filler addition system, at the same improve coating heat resistance,
Wearability and corrosion resistance;In the preparation process of modified manometer silicon dioxide, first with rare earth compound to nanometer titanium dioxide
Silicon is modified, and rare earth modified material A has been obtained, and is later modifying agent to material A using amino silicane coupling agent KH-550
It is modified, amino has been introduced into the surface of material A, obtained the material B for containing amino in surface;With material B and formaldehyde
Be that raw material is reacted with parahydroxyben-zaldehyde, by the condition of control reaction, make the amino of nano-silica surface with
Parahydroxyben-zaldehyde and formaldehyde are reacted, so that the polybenzoxazine structure containing aldehyde radical has been introduced into nano silica
Surface, improve the surface nature of nano silica, wherein introduce rare earth element, electronegativity is big, with organic coating
Compatibility it is good, be added in coating and be uniformly dispersed, and particle diameter distribution is wider, and the particle for facilitating different-grain diameter fills up the hole of coating
Gap reduces porosity, improves the corrosion resistance of coating, while introducing polybenzoxazine structure, paint solidification on its surface
During, crosslink density is high, and cure shrinkage is low, thermal stability is good, and during coating burns, carbon yield is high, improves
The anti-flammability of coating;It is solid trimellitic anhydride N-butyl, 2-ethyl-4-methylimidazole, zinc acrylate resin, boron amide class have been specifically chosen
The mixture of agent 594 cooperates as curing agent, four, reduces cured activation energy, is easier to carry out reaction,
In boron amine curing agent can promote anhydride group in trimellitic anhydride N-butyl open loop formed ion pair, push with it is epoxy curing
The progress of reaction, while it can consume epoxy group by cationic ring-opening polymerization, improve the curing rate of system, simultaneously
The mechanical property of coating can be improved in rigid six-membered cyclic structure in trimellitic anhydride N-butyl, avoids boron amine curing agent
The reduction of system fissipation factor tg δ value, maintains the intensity of coating caused by being added;In 1- pyrene butyric acid addition system, with oxidation
There is effect between graphene, improves dispersibility of the graphene oxide in system, further improve the heat resistance of coating
And corrosion resistance.
Specific embodiment
In the following, technical solution of the present invention is described in detail by specific embodiment.
Embodiment 1
A kind of nano-silicon dioxide modified epoxy coating proposed by the present invention, raw material includes: epoxy by weight
70 parts of resin, 8 parts of chlorinated rubber, 18 parts of silicone resin, 9 parts of alkyd resin, 3 parts of graphene oxide, 3 parts of nano silica,
8 parts of charcoal powder, 1 part of silicon carbide, nano-titanium are 1.8 parts black, 2 parts of precipitation method barium sulfate, 3 parts of bamboo fibre, 3 parts of basalt scale, receive
Rice 8 parts of aluminium oxide, 9 parts of curing agent, 1 part of 1- pyrene butyric acid, 20 parts of solvent, 1.5 parts of auxiliary agent;
Wherein, the curing agent is trimellitic anhydride N-butyl, 2-ethyl-4-methylimidazole, zinc acrylate resin, boron amide class are consolidated
The mixture of agent 594.
Embodiment 2
A kind of nano-silicon dioxide modified epoxy coating proposed by the present invention, raw material includes: epoxy by weight
55 parts of resin, 15 parts of chlorinated rubber, 5 parts of silicone resin, 15 parts of alkyd resin, 1 part of graphene oxide, 8 parts of nano silica,
2 parts of charcoal powder, 3 parts of silicon carbide, nano-titanium be 0.3 part black, 6 parts of precipitation method barium sulfate, 0.7 part of bamboo fibre, 9 parts of basalt scale,
2 parts of nano aluminium oxide, 25 parts of curing agent, 0.1 part of 1- pyrene butyric acid, 30 parts of solvent, 0.2 part of auxiliary agent;
Wherein, the curing agent is trimellitic anhydride N-butyl, 2-ethyl-4-methylimidazole, zinc acrylate resin, boron amide class are consolidated
The mixture of agent 594.
Embodiment 3
A kind of nano-silicon dioxide modified epoxy coating proposed by the present invention, raw material includes: epoxy by weight
68 parts of resin, 9 parts of chlorinated rubber, 16 parts of silicone resin, 11 parts of alkyd resin, 2.7 parts of graphene oxide, nano silica 4
Part, 7.2 parts of charcoal powder, 1.6 parts of silicon carbide, nano-titanium be 1.6 parts black, 3 parts of precipitation method barium sulfate, 2.7 parts of bamboo fibre, basalt squama
4 parts of piece, 7 parts of nano aluminium oxide, 11 parts of curing agent, 0.8 part of 1- pyrene butyric acid, 23 parts of solvent, 1.3 parts of auxiliary agent;
Wherein, the curing agent is trimellitic anhydride N-butyl, 2-ethyl-4-methylimidazole, zinc acrylate resin, boron amide class are consolidated
The mixture of agent 594;
The nano silica is modified manometer silicon dioxide;The modified manometer silicon dioxide according to following technique into
Row preparation: cetyl trimethylammonium bromide, sodium metasilicate, rare earth compound are mixed with distilled water, and pH value is adjusted after stirring and is
8,11h is stirred at normal temperature, and calcining obtains material A after standing, be filtered, washed, drying;It is to be modified with silane resin acceptor kh-550
Agent is modified material A, obtains material B;Material B, the formalin that mass fraction is 37% are mixed, it is anti-in ice-water bath
5h is answered, the toluene solution of parahydroxyben-zaldehyde is then added, 4h is reacted at 75 DEG C, washs after reaction, be dried to obtain institute
State modified manometer silicon dioxide;
In the preparation process of modified manometer silicon dioxide, cetyl trimethylammonium bromide, sodium metasilicate, rare earth compound
Weight ratio be 0.3:3:0.03;Silane resin acceptor kh-550, material A weight ratio be 0.7:1;Material B, mass fraction are
37% formalin, the weight ratio of parahydroxyben-zaldehyde are 1.4:0.7:1.5;
In the preparation process of modified manometer silicon dioxide, the temperature of calcining is 520 DEG C, time 3h;
In the preparation process of modified manometer silicon dioxide, the rare earth compound is holmium nitrate;
The graphene oxide is the graphene oxide of p-phenylenediamine functionalization;
The basalt scale is polyaniline-modified basalt scale;
The average grain diameter of the nano aluminium oxide is 85nm;
In curing agent, trimellitic anhydride N-butyl, 2-ethyl-4-methylimidazole, zinc acrylate resin, boron amine curing agent 594
Weight ratio be 2:1.2:0.5:1.7;
The auxiliary agent includes anti-settling agent, wetting dispersing agent, defoaming agent and levelling agent, and anti-settling agent, wetting dispersing agent, defoaming
The weight ratio of agent and levelling agent is 2.3:0.8:0.1:1.
Embodiment 4
A kind of nano-silicon dioxide modified epoxy coating proposed by the present invention, raw material includes: epoxy by weight
59 parts of resin, 14 parts of chlorinated rubber, 7 parts of silicone resin, 14 parts of alkyd resin, 1.8 parts of graphene oxide, nano silica 7
Part, 3 parts of charcoal powder, 2.7 parts of silicon carbide, nano-titanium be 0.5 part black, 5 parts of precipitation method barium sulfate, 0.9 part of bamboo fibre, basalt scale
8 parts, 3 parts of nano aluminium oxide, 22 parts of curing agent, 0.3 part of 1- pyrene butyric acid, 28 parts of solvent, 0.7 part of auxiliary agent;
Wherein, the curing agent is trimellitic anhydride N-butyl, 2-ethyl-4-methylimidazole, zinc acrylate resin, boron amide class are consolidated
The mixture of agent 594;
The nano silica is modified manometer silicon dioxide;The modified manometer silicon dioxide according to following technique into
Row preparation: cetyl trimethylammonium bromide, sodium metasilicate, rare earth compound are mixed with distilled water, and pH value is adjusted after stirring and is
9,8h is stirred at normal temperature, and calcining obtains material A after standing, be filtered, washed, drying;It is to be modified with silane resin acceptor kh-550
Agent is modified material A, obtains material B;Material B, the formalin that mass fraction is 37% are mixed, it is anti-in ice-water bath
7.5h is answered, the toluene solution of parahydroxyben-zaldehyde is then added, 6h is reacted at 60 DEG C, washs, be dried to obtain after reaction
The modified manometer silicon dioxide;
In the preparation process of modified manometer silicon dioxide, cetyl trimethylammonium bromide, sodium metasilicate, rare earth compound
Weight ratio be 0.5:2:0.08;Silane resin acceptor kh-550, material A weight ratio be 0.4:1;Material B, mass fraction are
37% formalin, the weight ratio of parahydroxyben-zaldehyde are 1.8:0.4:2.5;
In the preparation process of modified manometer silicon dioxide, the temperature of calcining is 490 DEG C, time 5h;
In the preparation process of modified manometer silicon dioxide, the rare earth compound is the mixture of erbium nitrate, samaric nitrate;
The graphene oxide is the graphene oxide of p-phenylenediamine functionalization;
The basalt scale is polyaniline-modified basalt scale;
The average grain diameter of the nano aluminium oxide is 30nm;
In curing agent, trimellitic anhydride N-butyl, 2-ethyl-4-methylimidazole, zinc acrylate resin, boron amine curing agent 594
Weight ratio be 5:0.1:2:1;
The auxiliary agent includes anti-settling agent, wetting dispersing agent, defoaming agent and levelling agent, and anti-settling agent, wetting dispersing agent, defoaming
The weight ratio of agent and levelling agent is 3.4:0.3:0.7:0.1.
Embodiment 5
A kind of nano-silicon dioxide modified epoxy coating proposed by the present invention, raw material includes: epoxy by weight
62 parts of resin, 11 parts of chlorinated rubber, 13 parts of silicone resin, 11 parts of alkyd resin, 2 parts of graphene oxide, nano silica 6
Part, 5 parts of charcoal powder, 2 parts of silicon carbide, nano-titanium be 1.5 parts black, 4.3 parts of precipitation method barium sulfate, 2.1 parts of bamboo fibre, basalt scale
5.3 parts, 5 parts of nano aluminium oxide, 17 parts of curing agent, 0.6 part of 1- pyrene butyric acid, 27 parts of solvent, 1 part of auxiliary agent;
Wherein, the curing agent is trimellitic anhydride N-butyl, 2-ethyl-4-methylimidazole, zinc acrylate resin, boron amide class are consolidated
The mixture of agent 594;
The nano silica is modified manometer silicon dioxide;The modified manometer silicon dioxide according to following technique into
Row preparation: cetyl trimethylammonium bromide, sodium metasilicate, rare earth compound are mixed with distilled water, and pH value is adjusted after stirring and is
8,10h is stirred at normal temperature, and calcining obtains material A after standing, be filtered, washed, drying;It is to be modified with silane resin acceptor kh-550
Agent is modified material A, obtains material B;Material B, the formalin that mass fraction is 37% are mixed, it is anti-in ice-water bath
6.7h is answered, the toluene solution of parahydroxyben-zaldehyde is then added, 5h is reacted at 68 DEG C, washs, be dried to obtain after reaction
The modified manometer silicon dioxide;
In the preparation process of modified manometer silicon dioxide, cetyl trimethylammonium bromide, sodium metasilicate, rare earth compound
Weight ratio be 0.4:2.7:0.05;Silane resin acceptor kh-550, material A weight ratio be 0.6:1;Material B, mass fraction are
37% formalin, the weight ratio of parahydroxyben-zaldehyde are 1.7:0.5:2.1;
In the preparation process of modified manometer silicon dioxide, the temperature of calcining is 500 DEG C, time 4h;
In the preparation process of modified manometer silicon dioxide, the rare earth compound is yttrium nitrate;
The graphene oxide is the graphene oxide of p-phenylenediamine functionalization;
The basalt scale is polyaniline-modified basalt scale;
The average grain diameter of the nano aluminium oxide is 70nm;
In curing agent, trimellitic anhydride N-butyl, 2-ethyl-4-methylimidazole, zinc acrylate resin, boron amine curing agent 594
Weight ratio be 3:1:1.7:1.5;
The auxiliary agent includes anti-settling agent, wetting dispersing agent, defoaming agent and levelling agent, and anti-settling agent, wetting dispersing agent, defoaming
The weight ratio of agent and levelling agent is 3:0.7:0.6:0.5.
Comparative example 1
With embodiment 5 only difference is that, do not add the modified manometer silicon dioxide in embodiment 5.
Comparative example 2
With embodiment 5 only difference is that, the modified manometer silicon dioxide in embodiment 5 is replaced with to common nanometer
Silica.
Comparative example 3
With embodiment 5 only difference is that, the modified manometer silicon dioxide in embodiment 5 is replaced with into existing silane
Coupling agent modified nano silica.
Comparative example 4
With embodiment 5 only difference is that, without containing the 1- pyrene butyric acid in embodiment 5.
It is tested using thermal stability of the thermogravimetric analysis to film in embodiment 5 and comparative example 1-4, as a result such as following table
It is shown:
Embodiment 5 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | |
Thermal decomposition temperature/DEG C | 287.8 | 201.5 | 221.3 | 229.7 | 248.9 |
Coating in embodiment 5 and comparative example 1-4 is corrosion-resistant coated in carrying out on the working electrode of Q235 steel matrix
Property test, corrosive medium be simulation oil water in field (wherein, sodium chloride concentration 17.55g/L, potassium chloride concentration 2.9g/L, chlorination
Calcium concentration is 5.5g/L, and sodium bicarbonate concentration is 0.53g/L, and solvent is water);Wherein, the corrosion current of embodiment 5 is 1.89 μ
A/cm2, the corrosion current of comparative example 1 is 9.1 μ A/cm2, the corrosion current of comparative example 2 is 4.57 μ A/cm2, the corrosion of comparative example 2
Electric current is 3.63 μ A/cm2, the corrosion current of comparative example 4 is 2.29 μ A/cm2。
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of nano-silicon dioxide modified epoxy coating, which is characterized in that its raw material includes: epoxy resin by weight
55-70 parts, 8-15 parts of chlorinated rubber, 5-18 parts of silicone resin, 9-15 parts of alkyd resin, 1-3 parts of graphene oxide, nano-silica
3-8 parts of SiClx, 2-8 parts of charcoal powder, 1-3 parts of silicon carbide, nano-titanium be 0.3-1.8 parts black, 2-6 parts of precipitation method barium sulfate, bamboo fibre
0.7-3 parts, 3-9 parts of basalt scale, 2-8 parts of nano aluminium oxide, 9-25 parts of curing agent, 0.1-1 parts of 1- pyrene butyric acid, solvent 20-
30 parts, 0.2-1.5 parts of auxiliary agent;
Wherein, the curing agent is trimellitic anhydride N-butyl, 2-ethyl-4-methylimidazole, zinc acrylate resin, boron amine curing agent
594 mixture.
2. nano-silicon dioxide modified epoxy coating according to claim 1, which is characterized in that the nanometer titanium dioxide
Silicon is modified manometer silicon dioxide;The modified manometer silicon dioxide is prepared according to following technique: by cetyl front three
Base ammonium bromide, sodium metasilicate, rare earth compound are mixed with distilled water, and it is 8-9 that pH value is adjusted after stirring, stir 8-11h at normal temperature,
Calcining obtains material A after standing, be filtered, washed, drying;Material A is modified using silane resin acceptor kh-550 as modifying agent,
Obtain material B;Material B, the formalin that mass fraction is 37% are mixed, 5-7.5h is reacted in ice-water bath, is then added
The toluene solution of parahydroxyben-zaldehyde reacts 4-6h at 60-75 DEG C, washs after reaction, is dried to obtain the modification and receives
Rice silica.
3. nano-silicon dioxide modified epoxy coating according to claim 2, which is characterized in that in modified nano-silica
In the preparation process of SiClx, cetyl trimethylammonium bromide, sodium metasilicate, rare earth compound weight ratio be 0.3-0.5:2-3:
0.03-0.08;Silane resin acceptor kh-550, material A weight ratio be 0.4-0.7:1;Material B, the first that mass fraction is 37%
Aldehyde solution, parahydroxyben-zaldehyde weight ratio be 1.4-1.8:0.4-0.7:1.5-2.5.
4. the nano-silicon dioxide modified epoxy coating according to Claims 2 or 3, which is characterized in that in modified Nano
In the preparation process of silica, the temperature of calcining is 490-520 DEG C, time 3-5h.
5. the nano-silicon dioxide modified epoxy coating according to any one of claim 2-4, which is characterized in that changing
Property nano silica preparation process in, the rare earth compound is holmium nitrate, erbium nitrate, samaric nitrate, one in yttrium nitrate
Kind or a variety of mixtures.
6. nano-silicon dioxide modified epoxy coating described in any one of -5 according to claim 1, which is characterized in that described
Graphene oxide is the graphene oxide of p-phenylenediamine functionalization.
7. nano-silicon dioxide modified epoxy coating described in any one of -6 according to claim 1, which is characterized in that described
Basalt scale is polyaniline-modified basalt scale.
8. nano-silicon dioxide modified epoxy coating described in any one of -7 according to claim 1, which is characterized in that described
The average grain diameter of nano aluminium oxide is 30-85nm.
9. nano-silicon dioxide modified epoxy coating described in any one of -8 according to claim 1, which is characterized in that solidification
In agent, trimellitic anhydride N-butyl, 2-ethyl-4-methylimidazole, zinc acrylate resin, boron amine curing agent 594 weight ratio be 2-
5:0.1-1.2:0.5-2:1-1.7.
10. nano-silicon dioxide modified epoxy coating described in any one of -9 according to claim 1, which is characterized in that institute
Stating auxiliary agent includes anti-settling agent, wetting dispersing agent, defoaming agent and levelling agent, and anti-settling agent, wetting dispersing agent, defoaming agent and levelling agent
Weight ratio be 2.3-3.4:0.3-0.8:0.1-0.7:0.1-1.
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CN111961397A (en) * | 2020-06-29 | 2020-11-20 | 安徽浩天新型材料有限公司 | Preparation method of high-temperature-resistant fireproof sleeve for cable |
CN115073950A (en) * | 2022-06-15 | 2022-09-20 | 苏州皇冠涂料科技发展有限公司 | Water-based environment-friendly high-weather-resistance anticorrosive paint and preparation method thereof |
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Application publication date: 20190503 |