CN103265661B - Coating and conductive resin of film zinc coat - Google Patents

Coating and conductive resin of film zinc coat Download PDF

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Publication number
CN103265661B
CN103265661B CN201310214888.4A CN201310214888A CN103265661B CN 103265661 B CN103265661 B CN 103265661B CN 201310214888 A CN201310214888 A CN 201310214888A CN 103265661 B CN103265661 B CN 103265661B
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graphene oxide
organic solvent
zinc
dropwise adding
hour
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CN103265661A (en
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廖有为
杨焰
车轶材
廖阳飞
王文
曾凡涌
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Hunan Jinpan New Material Science & Technology Co., Ltd.
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Hunan Jinpan New Material Science & Technology Co Ltd
Central South University of Forestry and Technology
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Abstract

The invention discloses a coating and conductive resin of a film zinc coat, which is prepared by the following steps of: weighing an organic solvent, methyl methacrylate, hydroxybutyl acrylate, hydroxyethyl methylacrylate, hydroxyethyl methacrylate phosphate, tert-butyl peroxy-2-ethylhexanoate and graphene oxide; adding 3/4 of the organic solvent and the graphene oxide into a reaction kettle A and mixing uniformly; uniformly mixing the methyl methacrylate, hydroxybutyl acrylate, hydroxyethyl methylacrylate, hydroxyethyl methacrylate phosphate and 3/4 of the tert-butyl peroxy-2-ethylhexanoate, dropwise adding the mixture into a dropwise adding tank B, and then dropwise adding into the reaction kettle A; uniformly mixing the residual organic solvent and tert-butyl peroxy-2-ethylhexanoate, dropwise adding the mixture into the dropwise adding tank B, then dropwise adding into the reaction kettle A at 113-118 DEG C, preserving heat for 0.8-1.2 hours, cooling and filtering; and performing ultrasonic treatment, adding hydrazine hydrate for reaction, filtering, washing and drying. The prepared film zinc coat has better corrosion resistance.

Description

Coated and the electroconductive resin that a kind of film is zinc-plated
Technical field
The present invention relates to the resin that a kind of film is zinc-plated, especially relate to the acrylate modified graphene coated of a kind of single-component and electroconductive resin.
Background technology
The product (market being also referred to as Zinc-base plating or cold galvanizing product) that film is zinc-plated; novel with it, long-acting, environmental protection, easily anticorrosion of steel structure technology are especially in steel construction maintenance; represent outstanding advantage; it not only inherits that traditional electrical is zinc-plated, the advantage of hot spray painted zinc and zinc-rich paint; and overcome their deficiency; dry film metallic zinc content up to more than 96%, can have galvanic protection and barrier protection double protection, has a good application prospect.
But existing film galvanizing production, due to selection and the resin-coated zinc powder technology existing defects of resin, make the specific conductivity of film galvanizing production not enough, initiatively galvanic protection effect is small and weak, and antiseptic property still owes desirable.
Summary of the invention
Technical problem to be solved by this invention is, provides the coated and electroconductive resin that the better film of a kind of antiseptic property is zinc-plated.
The technical solution adopted for the present invention to solve the technical problems is: the coated and electroconductive resin that a kind of film is zinc-plated, is made up of following methods:
(1) preparation of graphene oxide/acrylate copolymer
A. each component raw material is taken by following percent mass proportioning: organic solvent 30-50%, methyl methacrylate 30-50%, hy-droxybutyl 5-10%, hydroxyethyl methylacrylate 5-10%, functional monomer hydroxyethyl methacrylic acid phosphoric acid salt 2-4%, initiator peroxide-2 ethyl hexanoic acid tert-butyl ester 1-3%, graphene oxide 0.5-1.5%; Described each component per distribution ratio sum is 100%;
B. the organic solvent of taken formula ratio 70-80wt%, graphene oxide are added in reactor A, stir;
C., after the initiator peroxide-2 ethyl hexanoic acid tert-butyl ester of taken methyl methacrylate, hy-droxybutyl, hydroxyethyl methylacrylate, functional monomer hydroxyethyl methacrylic acid phosphoric acid salt, formula ratio 70-80wt% being mixed, add in dropwise adding tank B;
D. under whipped state, drop in reactor A in 105-112 DEG C by the mix monomer in dropwise adding tank B, control time for adding is 2.5-3.5 hour, after dripping, is warming up to 113-118 DEG C, insulation 0.8-1.2 hour;
E. after remaining organic solvent and initiator peroxide-2 ethyl hexanoic acid tert-butyl ester being mixed, join in dropwise adding tank B, drop in reactor A in 113-118 DEG C, control time for adding is 0.8-1.2 hour, after dripping, insulation 0.8-1.2 hour, is then cooled to 65-75 DEG C, filter discharging, obtain graphene oxide/acrylate copolymer;
(2) preparation of acrylate modified Graphene resin
F. by step e gained graphene oxide/acrylate copolymer supersound process 25-40 minute, then add weight and be equivalent to graphene oxide/acrylate copolymer 0.2-0.5 50-55wt% hydrazine hydrate doubly, in 85-95 DEG C of isothermal reaction 9-12 hour, filter, with deionized water wash filter cake 3-5 time, dry 22-25 hour at 55-65 DEG C again.
Further, in step a, the percent mass proportioning of each component raw material is: organic solvent 32-40%, methyl methacrylate 41-47%, hy-droxybutyl 7-9%, hydroxyethyl methylacrylate 6-8%, functional monomer hydroxyethyl methacrylic acid phosphoric acid salt 2.5-3.5%, initiator peroxide-2 ethyl hexanoic acid tert-butyl ester 1.5-2.5%, graphene oxide 0.8-1.2%; Preferred organic solvent 35%, methyl methacrylate 44%, hy-droxybutyl 8%, hydroxyethyl methylacrylate 7%, functional monomer hydroxyethyl methacrylic acid phosphoric acid salt 3%, initiator peroxide-2 ethyl hexanoic acid tert-butyl ester 2%, graphene oxide 1%.
Further, in step a, described organic solvent is dimethylbenzene.
Further, in step f, add 50-55wt% hydrazine hydrate weight be equivalent to 1/3 of graphene oxide/acrylate copolymer.
Research shows, the basic structural unit of Graphene is benzene six-ring the most stable in organic materials, is current optimal two-dimension nano materials.Desirable graphene-structured is plane hexagonal lattice, can be regarded as the graphitic molecules that one deck is stripped, each carbon atom is sp2 hydridization, and contributes the electronics on residue p track to form large π key, π-electron can move freely, and gives the electroconductibility that Graphene is good.Simultaneously due to this two-sided aromatic hydrocarbon structure of Graphene, (theoretical value is 2630m to make its specific surface area having super large 2/ g), therefore, there is high loading capacity, make it become very potential coating material.
Adding of Graphene, resin-coated electroconductibility and the snappiness of film zinc-plated (Zinc-base plating or cold galvanizing) can be given.Because the connection in Graphene between each carbon atom is very pliable and tough, when applying external mechanical force, carbon atom face with regard to flexural deformation, thus makes carbon atom need not rearrange to adapt to external force, also just maintains Stability Analysis of Structures.The interference that this stable crystalline network makes its electronics be subject to is very little, thus makes carbon atom have outstanding electroconductibility.Because Graphene is a kind of individual layer sheetlike material be made up of carbon atom, be all that carbon atom does not have functional group substantially above it, so Graphene can not directly with acrylic ester grafted.But the precursor of Graphene---graphene oxide ratio is easier to carry out with acrylate grafting, the chemical reaction such as coated, and this mainly make use of the abundant highly active oxygen-containing functional group such as carboxyl, carbonyl, hydroxyl of surface of graphene oxide.But in oxidising process, the conjugate network of graphite flake layer is subject to serious functionalized impact, makes graphene oxide almost lose electroconductibility.So the graphene oxide/acrylate compound material require hydrazine hydrate after graft copolymerization carries out reducing to recover its electroconductibility.
Compared with prior art, the present invention has the following advantages:
(1) add functional monomer hydroxyethyl methacrylic acid phosphoric acid salt, greatly can improve resin to the coated of zinc powder and the attachment to base material; Because selection has the organic resin of some functional group (hydroxyl, amino, phosphate anion etc.) or these have the resin of functional group by interpolation, making them form chemical bond on zinc particle surface is formed firmly coated, and hydroxyethyl methacrylic acid phosphoric acid salt contains high-content hydroxyl (-OH) and phosphate anion isopolarity group, be conducive to the attachment to matrix metal;
(2) introduce Graphene in the mode of graphene oxide, be conducive to improving the zinc-plated electroconductibility of film; Because if organic resin is carried out entirely coated to zinc powder, shielding will be given the electroconductibility of zinc powder, this just makes the zinc-plated zinc powder of film and steel substrate not form galvanic cell, zinc powder can not " sacrificial anode ", thus just can not protect steel substrate, but because resin is electroconductive resin, the conduction zinc fine particles of keeping apart is contacted each other again and forms the unlimited network chain of a kind of conduction, the conduction of the zinc-plated system of final film is unaffected, film zinc coating still can be conducted electricity, antiseptic principle and electro-galvanizing suitable;
(3) can with steel surface on form hydrogen bond, the Van der Waals force that formed much larger than secondary valence bond of reactive force that hydrogen bond produces, is conducive to coating and is combined with base material; In addition surface of steel plate sandblasting, matrix roughness can be improved, make zinc coating and matrix better " engagement ", there is anchoring effect, make zinc particle be attached on matrix firmly like this, produce the metallic bond reactive force that bonding strength is higher, make that film is zinc-plated with metallic surface, electrochemistry to be occurred and be combined, strong adhesion antistripping, therefore, film zinc coating has excellent sticking power to sandblasting plate;
(4) in hardness, snappiness and resistance to impact shock etc., excellent physicals is shown; Because the connection in Graphene between each carbon atom is very pliable and tough, when applying external mechanical force, carbon atom face with regard to flexural deformation, thus makes this resin have extremely strong toughness, and meanwhile, the Tg value of this resin comparatively, has higher hardness.
The film utilizing resin-made of the present invention to obtain is zinc-plated, and its antiseptic property is better, and salt spray resistance reaches more than 9600 hours, simultaneously every excellent combination property such as hardness, snappiness, shock resistance and sticking power.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
Coated and the electroconductive resin that the film of the present embodiment is zinc-plated, be made up of following methods:
(1) preparation of graphene oxide/acrylate copolymer
A. organic solvent dimethylbenzene 350kg is taken, methyl methacrylate 440kg, hy-droxybutyl 80kg, hydroxyethyl methylacrylate 70kg, functional monomer hydroxyethyl methacrylic acid phosphoric acid salt 30kg, initiator peroxide-2 ethyl hexanoic acid tert-butyl ester 20kg, graphene oxide 10kg;
B. the organic solvent of taken formula ratio 75wt%, graphene oxide are added in reactor A, stir;
C., after the initiator peroxide-2 ethyl hexanoic acid tert-butyl ester of taken methyl methacrylate, hy-droxybutyl, hydroxyethyl methylacrylate, functional monomer hydroxyethyl methacrylic acid phosphoric acid salt, formula ratio 75wt% being mixed, add in dropwise adding tank B;
D. under whipped state, drop in reactor A in 110 ± 1 DEG C by the mix monomer in dropwise adding tank B, time for adding is 3 hours, after dripping, and is warming up to 115 DEG C, is incubated 1 hour;
E. after remaining organic solvent and initiator peroxide-2 ethyl hexanoic acid tert-butyl ester being mixed, join in dropwise adding tank B, drop in reactor A in 115 DEG C, time for adding is 1 hour, after dripping, be incubated 1 hour, be then cooled to 70 DEG C, filter discharging, obtain 1000kg graphene oxide/acrylate copolymer;
(2) preparation of acrylate modified Graphene resin
F. by step e gained graphene oxide/acrylate copolymer supersound process 30 minutes, then the 51.2wt% hydrazine hydrate that weight is equivalent to graphene oxide/acrylate copolymer 1/3 is added, in 90 DEG C of isothermal reactions 10 hours, filter, with deionized water wash filter cake 4 times, at 60 DEG C dry 24 hours again.
The glass transition temperature Tg of this resin is 80, and acid number is less than 1mgKOH/g.
Embodiment 2
Coated and the electroconductive resin that the film of the present embodiment is zinc-plated, be made up of following methods:
(1) preparation of graphene oxide/acrylate copolymer
A. organic solvent dimethylbenzene 400kg is taken, methyl methacrylate 350kg, hy-droxybutyl 100kg, hydroxyethyl methylacrylate 100kg, functional monomer hydroxyethyl methacrylic acid phosphoric acid salt 20kg, initiator peroxide-2 ethyl hexanoic acid tert-butyl ester 15kg, graphene oxide 15kg;
B. the organic solvent of taken formula ratio 75wt%, graphene oxide are added in reactor A, stir;
C., after the initiator peroxide-2 ethyl hexanoic acid tert-butyl ester of taken methyl methacrylate, hy-droxybutyl, hydroxyethyl methylacrylate, functional monomer hydroxyethyl methacrylic acid phosphoric acid salt, formula ratio 75wt% being mixed, add in dropwise adding tank B;
D. under whipped state, drop in reactor A in 110 ± 1 DEG C by the mix monomer in dropwise adding tank B, time for adding is 3 hours, after dripping, and is warming up to 115 DEG C, is incubated 1 hour;
E. after remaining organic solvent and initiator peroxide-2 ethyl hexanoic acid tert-butyl ester being mixed, join in dropwise adding tank B, drop in reactor A in 115 DEG C, time for adding is 1 hour, after dripping, be incubated 1 hour, be then cooled to 70 DEG C, filter discharging, obtain 1000kg graphene oxide/acrylate copolymer;
(2) preparation of acrylate modified Graphene resin
F. by step e gained graphene oxide/acrylate copolymer supersound process 30 minutes, then the 51.2wt% hydrazine hydrate that weight is equivalent to graphene oxide/acrylate copolymer 1/3 is added, in 90 DEG C of isothermal reactions 10 hours, filter, with deionized water wash filter cake 4 times, at 60 DEG C dry 24 hours again.
The glass transition temperature Tg of this resin is 60, and acid number is less than 0.5mgKOH/g.
Embodiment 3
Coated and the electroconductive resin that the film of the present embodiment is zinc-plated, be made up of following methods:
(1) preparation of graphene oxide/acrylate copolymer
A. organic solvent dimethylbenzene 300kg is taken, methyl methacrylate 500kg, hy-droxybutyl 50kg, hydroxyethyl methylacrylate 80kg, functional monomer hydroxyethyl methacrylic acid phosphoric acid salt 40kg, initiator peroxide-2 ethyl hexanoic acid tert-butyl ester 25kg, graphene oxide 5kg;
B. the organic solvent of taken formula ratio 75wt%, graphene oxide are added in reactor A, stir;
C., after the initiator peroxide-2 ethyl hexanoic acid tert-butyl ester of taken methyl methacrylate, hy-droxybutyl, hydroxyethyl methylacrylate, functional monomer hydroxyethyl methacrylic acid phosphoric acid salt, formula ratio 75wt% being mixed, add in dropwise adding tank B;
D. under whipped state, drop in reactor A in 110 ± 1 DEG C by the mix monomer in dropwise adding tank B, time for adding is 3 hours, after dripping, and is warming up to 115 DEG C, is incubated 1 hour;
E. after remaining organic solvent and initiator peroxide-2 ethyl hexanoic acid tert-butyl ester being mixed, join in dropwise adding tank B, drop in reactor A in 115 DEG C, time for adding is 1 hour, after dripping, be incubated 1 hour, be then cooled to 70 DEG C, filter discharging, obtain 1000kg graphene oxide/acrylate copolymer;
(2) preparation of acrylate modified Graphene resin
F. by step e gained graphene oxide/acrylate copolymer supersound process 30 minutes, then the 51.2wt% hydrazine hydrate that weight is equivalent to graphene oxide/acrylate copolymer 1/3 is added, in 90 DEG C of isothermal reactions 10 hours, filter, with deionized water wash filter cake 4 times, at 60 DEG C dry 24 hours again.
The glass transition temperature Tg of this resin is 90, and acid number is less than 2mgKOH/g.
The resin method of inspection
First coated, the electroconductive resin (acrylate modified Graphene resin) of zinc-plated for above-mentioned film (Zinc-base plating or cold galvanizing) is dissolved into after solid part is the resin liquid of 50wt% with the mixed solvent that n-butyl acetate, 2-Butoxyethyl acetate, S-200 industrial naptha mass ratio are 1:4:1 respectively, then prepares film zinc-plated (Zinc-base plating or cold galvanizing) anticorrosive.Test its every salient features.
It is as follows that it detects its performance:

Claims (5)

1. the coated and electroconductive resin that film is zinc-plated, is characterized in that, be made up of following methods:
(1) preparation of graphene oxide/acrylate copolymer
A. each component raw material is taken by following percent mass proportioning: organic solvent 30-50%, methyl methacrylate 30-50%, hy-droxybutyl 5-10%, hydroxyethyl methylacrylate 5-10%, functional monomer hydroxyethyl methacrylic acid phosphoric acid salt 2-4%, initiator t butyl 2 ethyl peroxyhexanoate 1-3%, graphene oxide 0.5-1.5%; Described each component per distribution ratio sum is 100%;
B. the organic solvent of taken formula ratio 70-80wt%, graphene oxide are added in reactor A, stir;
C., after the initiator t butyl 2 ethyl peroxyhexanoate of taken methyl methacrylate, hy-droxybutyl, hydroxyethyl methylacrylate, functional monomer hydroxyethyl methacrylic acid phosphoric acid salt, formula ratio 70-80wt% being mixed, add in dropwise adding tank B;
D. under whipped state, drop in reactor A in 105-112 DEG C by the mix monomer in dropwise adding tank B, control time for adding is 2.5-3.5 hour, after dripping, is warming up to 113-118 DEG C, insulation 0.8-1.2 hour;
E. after remaining organic solvent and initiator t butyl 2 ethyl peroxyhexanoate being mixed, join in dropwise adding tank B, drop in reactor A in 113-118 DEG C, control time for adding is 0.8-1.2 hour, after dripping, insulation 0.8-1.2 hour, is then cooled to 65-75 DEG C, filter discharging, obtain graphene oxide/acrylate copolymer;
(2) preparation of acrylate modified Graphene resin
F. by step e gained graphene oxide/acrylate copolymer supersound process 25-40 minute, then add weight and be equivalent to graphene oxide/acrylate copolymer 0.2-0.5 50-55wt% hydrazine hydrate doubly, in 85-95 DEG C of isothermal reaction 9-12 hour, filter, with deionized water wash filter cake 3-5 time, dry 22-25 hour at 55-65 DEG C again.
2. the coated and electroconductive resin that film according to claim 1 is zinc-plated, it is characterized in that: in step a, the percent mass proportioning of each component raw material is: organic solvent 32-40%, methyl methacrylate 41-47%, hy-droxybutyl 7-9%, hydroxyethyl methylacrylate 6-8%, functional monomer hydroxyethyl methacrylic acid phosphoric acid salt 2.5-3.5%, initiator t butyl 2 ethyl peroxyhexanoate 1.5-2.5%, graphene oxide 0.8-1.2%.
3. the coated and electroconductive resin that film according to claim 2 is zinc-plated, it is characterized in that: in step a, the percent mass proportioning of each component raw material is: organic solvent 35%, methyl methacrylate 44%, hy-droxybutyl 8%, hydroxyethyl methylacrylate 7%, functional monomer hydroxyethyl methacrylic acid phosphoric acid salt 3%, initiator t butyl 2 ethyl peroxyhexanoate 2%, graphene oxide 1%.
4. the coated and electroconductive resin that the film according to claim 1 or 2 or 3 is zinc-plated, it is characterized in that: in step a, described organic solvent is dimethylbenzene.
5. the coated and electroconductive resin that the film according to claim 1 or 2 or 3 is zinc-plated, is characterized in that: in step f, add 50-55wt% hydrazine hydrate weight be equivalent to 1/3 of graphene oxide/acrylate copolymer.
CN201310214888.4A 2013-06-03 2013-06-03 Coating and conductive resin of film zinc coat Active CN103265661B (en)

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CN104130602A (en) * 2014-07-16 2014-11-05 奉化市宇创产品设计有限公司 Cold spraying nickel coating and preparation method thereof
TWI555803B (en) * 2014-07-31 2016-11-01 中原大學 Ananticorrosive layer having a biomimetic leaf surface nano-microstructure and the application thereof
CN106479285A (en) * 2016-09-12 2017-03-08 中国航空工业集团公司北京航空材料研究院 A kind of Graphene strengthens waterborne rusted paint and its preparation and application
CN106497301B (en) * 2016-10-17 2018-09-14 哈尔滨工业大学无锡新材料研究院 A kind of graphene modification acrylate antistatic film and preparation method thereof
CN106947983B (en) * 2017-03-31 2019-06-18 湖南金磐新材料科技有限公司 Intercalation Zn-Al alloy powder and its zinc-aluminium of preparation collaboration anticorrosive paint and method
CN107805442B (en) * 2017-11-14 2020-01-31 青岛爱尔家佳新材料股份有限公司 Graphene modified water-based anticorrosive paint and preparation method thereof

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