CN105713481A - Graphene-modified epoxy zinc-rich primer and preparation method thereof - Google Patents
Graphene-modified epoxy zinc-rich primer and preparation method thereof Download PDFInfo
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- CN105713481A CN105713481A CN201410725574.5A CN201410725574A CN105713481A CN 105713481 A CN105713481 A CN 105713481A CN 201410725574 A CN201410725574 A CN 201410725574A CN 105713481 A CN105713481 A CN 105713481A
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Abstract
The invention relates to graphene-modified epoxy zinc-rich primer and a preparation method thereof. The graphene-modified epoxy zinc-rich primer comprises, by mass, 15-30 parts of modified epoxy resin, 0.3-5 parts of graphene, 2-8 parts of butanol, 4-10 parts of toluene, 0.3-3 parts of an anti-settling agent and 70-90 parts of zinc dust and the modified epoxy resin is phthalic acid-modified epoxy resin. The preparation method comprises 1, preparing modified epoxy resin which is phthalic acid-modified epoxy resin, 2, preparing graphene epoxy resin slurry and 3, preparing the graphene-modified epoxy zinc-rich primer. Through a reaction of modified epoxy resin hydroxyl and phthalic anhydride, high polarity carboxyl is introduced so that the epoxy resin forms a dispersant with a very strong dispersion capability and can efficiently disperse and chelate graphene so that graphene and resin are chelated and are uniformly dispersed in a paint system and optimal anticorrosion effects are obtained. Through a sheet structure of graphene, a paint film is compact, a corrosive gas entrance path is extended and anticorrosion effects are further improved.
Description
Technical field
The present invention relates to a kind of coating composition and preparation method thereof, particularly to a kind of epoxy zinc rich primer and preparation method thereof.
Background technology
Epoxy zinc rich primer is with epoxy resin, zinc powder for primary raw material; the sapecial coating of the composition such as filler, auxiliary agent, solvent; its antiseptic property is excellent; attached outstanding power is strong; in paint film, zinc content is high; having cathodic protection effect, water resistance is excellent, it is adaptable to the priming coat etc. of storage tank, container, steel construction, steel pipe, ocean platform, boats and ships, harbour facility and severe anticorrosion environment.
Graphene is the new material of a kind of monolayer laminated structure being made up of carbon atom.It is a kind of formed the flat film that hexangle type is honeycomb lattice, the two-dimensional material of only one of which carbon atom thickness by carbon atom with sp2 hybrid orbital.The nano material that world that Graphene is known is thin, the hardest, it is almost fully transparent, only absorbs the light of 2.3%；Heat conductivity is up to 5300W/m K, and higher than CNT and diamond, under room temperature, its electron mobility is more than 15000cm2/V s, again ratio CNT or silicon wafer height, and resistivity only about 10-8 Ω m, lower than copper or silver, for the material that world resistivity is minimum.
Chinese patent application 201310538981.0, name is called a kind of high-temperature resistant anti-corrosive based on Graphene and preparation method thereof, and this patent fire-resistant anticorrosion paint consists of: epoxy resin 5-60%, polyphenylene sulfide 3-30%.Amino resins 3-30%, pigment 1-10%, Graphene 1-20%, n-butyl alcohol 3-50%, defoamer 0.1-0.3%, poly-hydroxy acid sodium salt 0.1-10%, dibutyl phthalate 0.1-5%, bentonite 0.5-1.0%, levelling agent 0.2-0.5%.First preparation method for join in n-butyl alcohol by Graphene, epoxy resin, polyphenylene sulfide, and ultrasonic agitation, then by other raw materials addition grinding machine for grinding, finally by the two stirring mixing.
Chinese patent application 201410097011.6, name is called zinc alkene anticorrosive paint and preparation method thereof, and this coating includes component A and B component, and B component is firming agent.Component A includes Graphene epoxy resin solution 10-20%, anti-settling agent 0.5-2%, zinc powder 15-30%, aluminium powder 2-10%, antirust color stuffing 35-50%, organic solvent 5-10%.Graphene epoxy resin solution comprises Graphene 1-10%, epoxy resin liquid 80-90%, organic solvent 5-10%, auxiliary agent 1-2%.First prepare Graphene epoxy resin liquid during preparation, namely with organic solvent and auxiliary agent pre-preg Graphene, use organic solvent dissolution epoxy resin simultaneously, then pre-preg Graphene is joined mix homogeneously in the epoxy resin liquid dissolved.
Graphene is prone to when using in coating assemble, and is not easily uniformly dispersed in system, ultrasonic agitation or pre-preg in above-mentioned prior art, all adopts the mode of physics can not solve the problem disperseing inequality of Graphene very well.
Summary of the invention
It is an object of the invention to: solve deficiency of the prior art, it is provided that a kind of Graphene modified epoxy zinc rich primer and preparation method thereof.
The technical scheme realizing the object of the invention is: a kind of Graphene modified epoxy zinc rich primer, and each constituent mass number is:
Modified epoxy 15～30 parts, it is preferable that 15,16,17,18,19,20,21,22,23,24,25,26,27,28,29,30 parts；Graphene 0.3～5 part, it is preferable that 0.3,0.4,0.5,0.6,0.7,0.8,0.9,1.0,1.2,1.4,1.5,1.6,1.8,2.0,2.2,2.4,2.5,2.6,2.8,3.0,3.5,4.0,4.5,5.0 parts；2～8 parts of butanol, it is preferable that 2,3,4,5,6,7,8 parts；Toluene 4～10 parts, it is preferable that 4,5,6,7,8,9,10 parts；Anti-settling agent 0.3～3 part, it is preferable that 0.3,0.4,0.5,0.6,0.7,0.8,0.9,1.0,1.5,2.0,2.5,3.0；Zinc powder 70～90 parts, it is preferable that 70,75,80,85,88,90 parts；Described modified epoxy is orthophthalic modified epoxy resin.
Graphene modified epoxy zinc rich primer of the present invention, it is preferable that each constituent mass number is: modified epoxy 19 parts；Graphene 0.5～3 part；4 parts of butanol；Toluene 6 parts；Anti-settling agent 0.5 part；Zinc powder 85 parts.
Graphene modified epoxy zinc rich primer of the present invention, it is preferable that each constituent mass number is: modified epoxy 25 parts；Graphene 0.5～5 part；5 parts of butanol；Toluene 8 parts；Anti-settling agent 0.8 part；Zinc powder 88 parts.
Raw material epoxy resin of the present invention is preferably Commercial epoxy resins SM6101.
The preparation method of Graphene modified epoxy zinc rich primer of the present invention, including:
Step (1) prepares the orthophthalic modified epoxy resin of modified epoxy:
Epoxy resin is put into reactor, is heated with stirring to 70-90 DEG C, it is preferable that 80 DEG C, put into phthalic anhydride, continue stirring, 70-90 DEG C, it is preferable that cool down after 80 DEG C of insulation reaction, namely prepare phthalic acid epoxy resin；Reaction equation is
Step (2) prepares Graphene epoxy resin grout:
The phthalic acid epoxy resin step (1) prepared puts in a mixing bowl, adds Graphene high-speed stirred half an hour, uniformly pasty state, namely prepares Graphene epoxy resin grout；
Step (3) prepares Graphene modified epoxy zinc rich primer:
Graphene epoxy resin grout prepared by step (2) adds, is slowly stirred while put into more than toluene, butanol, anti-settling agent, zinc powder, then high speed dispersion half an hour successively, regulates viscosity, prepare Graphene modified epoxy zinc rich primer.
The preparation method of above-mentioned Graphene modified epoxy zinc rich primer, wherein the addition of step (1) phthalic anhydride is the 1%～15% of epoxy resin quality, it is preferable that 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%.
The present invention has positive effect: (1) is by the modified epoxy hydroxyl by epoxy resin and phthalic anhydride reaction, the phthalic acid epoxy resin generated is owing to introducing highly polar carboxyl, epoxy resin has inherently become the dispersant that dispersibility is extremely strong, can disperse efficiently and chelating Graphene, make Graphene and resin chelating, it is evenly dispersed in coating system, reaches best antiseptic effect；(2) laminated structure of Graphene makes paint film finer and close, and the path of etchant gas entrance is elongated further enhances anti-corrosion effects.
Detailed description of the invention
(embodiment 1)
One, the orthophthalic modified epoxy resin of modified epoxy is prepared:
Epoxy resin 100Kg is put into reactor, is heated with stirring to 80 DEG C, put into phthalic anhydride 5Kg, continue stirring, 80 DEG C of insulations cooling in 15 minutes, namely prepare phthalic acid epoxy resin.
Two, Graphene epoxy resin grout is prepared:
The phthalic acid epoxy resin 19Kg that step (1) prepared puts in a mixing bowl, adds Graphene 0.5Kg high-speed stirred half an hour, uniformly pasty state, namely prepares Graphene epoxy resin grout；
Three, Graphene modified epoxy zinc rich primer is prepared:
Low rate mixing again, puts into solvent toluene 6Kg, butanol 4Kg, anti-settling agent organobentonite 0.5Kg, zinc powder 85Kg, high speed dispersion half an hour successively, regulates viscosity, filter and prepare epoxy zinc rich primer.
When coating uses, first component is epoxy zinc rich primer, and component B is the phenolic aldehyde amine (i.e. T-31) of 30%, first component: component B=10:1.
(embodiment 2)
One, the orthophthalic modified epoxy resin of modified epoxy is prepared:
Epoxy resin 100Kg is put into reactor, is heated with stirring to 80 DEG C, put into phthalic anhydride 8Kg, continue stirring, 80 DEG C of insulations cooling in 15 minutes, namely prepare phthalic acid epoxy resin.
Two, Graphene epoxy resin grout is prepared:
The phthalic acid epoxy resin 25Kg that step (1) prepared puts in a mixing bowl, adds Graphene 0.8Kg high-speed stirred half an hour, uniformly pasty state, namely prepares Graphene epoxy resin grout；
Three, Graphene modified epoxy zinc rich primer is prepared:
Low rate mixing again, puts into solvent toluene 8Kg, butanol 5Kg, anti-settling agent polyamide wax 0.8Kg, zinc powder 88Kg, high speed dispersion half an hour successively, regulates viscosity, filter and prepare epoxy zinc rich primer.
When coating uses, first component is epoxy zinc rich primer, and component B is the phenolic aldehyde amine (i.e. T-31) of 30%, first component: component B=10:1.
(embodiment 3)
One, the orthophthalic modified epoxy resin of modified epoxy is prepared:
Epoxy resin 100Kg is put into reactor, is heated with stirring to 80 DEG C, put into phthalic anhydride 10Kg, continue stirring, 85 DEG C of insulations cooling in 15 minutes, namely prepare phthalic acid epoxy resin.
Two, Graphene epoxy resin grout is prepared:
The phthalic acid epoxy resin 16Kg that step (1) prepared puts in a mixing bowl, adds Graphene 1.1Kg high-speed stirred half an hour, uniformly pasty state, namely prepares Graphene epoxy resin grout；
Three, Graphene modified epoxy zinc rich primer is prepared:
Low rate mixing again, puts into solvent toluene 7Kg, butanol 3Kg, anti-settling agent polyamide wax 0.6Kg, zinc powder 75Kg, high speed dispersion half an hour successively, regulates viscosity, filter and prepare epoxy zinc rich primer.
When coating uses, first component is epoxy zinc rich primer, and component B is the phenolic aldehyde amine (i.e. T-31) of 30%, first component: component B=10:1.
(embodiment 4)
One, the orthophthalic modified epoxy resin of modified epoxy is prepared:
Epoxy resin 100Kg is put into reactor, is heated with stirring to 80 DEG C, put into phthalic anhydride 11Kg, continue stirring, 88 DEG C of insulations cooling in 15 minutes, namely prepare phthalic acid epoxy resin.
Two, Graphene epoxy resin grout is prepared:
The phthalic acid epoxy resin 22Kg that step (1) prepared puts in a mixing bowl, adds Graphene 1.5Kg high-speed stirred half an hour, uniformly pasty state, namely prepares Graphene epoxy resin grout；
Three, Graphene modified epoxy zinc rich primer is prepared:
Low rate mixing again, puts into solvent toluene 6Kg, butanol 6Kg, anti-settling agent organobentonite 1.5Kg, zinc powder 80Kg, high speed dispersion half an hour successively, regulates viscosity, filter and prepare epoxy zinc rich primer.
When coating uses, first component is epoxy zinc rich primer, and component B is the phenolic aldehyde amine (i.e. T-31) of 30%, first component: component B=10:1.
(embodiment 5)
One, the orthophthalic modified epoxy resin of modified epoxy is prepared:
Epoxy resin 100Kg is put into reactor, is heated with stirring to 80 DEG C, put into phthalic anhydride 13Kg, continue stirring, 76 DEG C of insulations cooling in 30 minutes, namely prepare phthalic acid epoxy resin.
Two, Graphene epoxy resin grout is prepared:
The phthalic acid epoxy resin 27Kg that step (1) prepared puts in a mixing bowl, adds Graphene 4.5Kg high-speed stirred half an hour, uniformly pasty state, namely prepares Graphene epoxy resin grout；
Three, Graphene modified epoxy zinc rich primer is prepared:
Low rate mixing again, puts into solvent toluene 8Kg, butanol 9Kg, anti-settling agent organobentonite 2.6Kg, zinc powder 90Kg, high speed dispersion half an hour successively, regulates viscosity, filter and prepare epoxy zinc rich primer.
When coating uses, first component is epoxy zinc rich primer, and component B is the phenolic aldehyde amine (i.e. T-31) of 30%, first component: component B=10:1.
Applying the Graphene epoxy zinc rich primer epoxy zinc rich primer traditional with the Zn content that communicates that preparation technology of the present invention produces to compare salt fog resistance and significantly improve, testing result is as follows:
Particular embodiments described above; the purpose of the present invention, technical scheme and beneficial effect have been further described; it is it should be understood that; the foregoing is only specific embodiments of the invention; it is not limited to the present invention; all within the spirit and principles in the present invention, any amendment of making, equivalent replacement, improvement etc., should be included within protection scope of the present invention.
Claims (7)
1. a Graphene modified epoxy zinc rich primer, it is characterised in that each constituent mass number is:
Described modified epoxy is orthophthalic modified epoxy resin.
2. Graphene modified epoxy zinc rich primer according to claim 1, it is characterised in that each constituent mass number is:
3. Graphene modified epoxy zinc rich primer according to claim 1, it is characterised in that each constituent mass number is:
4. the Graphene modified epoxy zinc rich primer according to claim 1 or 2 or 3, it is characterised in that: the epoxy resin of described orthophthalic modified epoxy resin is epoxy resin SM6101.
5. one kind as arbitrary in Claims 1 to 4 as described in the preparation method of Graphene modified epoxy zinc rich primer, it is characterised in that: including:
Step (1) prepares the orthophthalic modified epoxy resin of modified epoxy:
Epoxy resin is put into reactor, is heated with stirring to 70-90 DEG C, put into phthalic anhydride, continue stirring, cool down after 70-90 DEG C of insulation reaction, namely prepare phthalic acid epoxy resin；
Step (2) prepares Graphene epoxy resin grout:
The phthalic acid epoxy resin step (1) prepared puts in a mixing bowl, adds more than Graphene high-speed stirred half an hour, uniformly pasty state, namely prepares Graphene epoxy resin grout；
Step (3) prepares Graphene modified epoxy zinc rich primer:
Graphene epoxy resin grout prepared by step (2) adds, is slowly stirred while put into more than toluene, butanol, anti-settling agent, zinc powder, then high speed dispersion half an hour successively, regulates viscosity, prepare Graphene modified epoxy zinc rich primer.
6. the preparation method of Graphene modified epoxy zinc rich primer according to claim 5, it is characterised in that: wherein the addition of step (1) phthalic anhydride is the 1%～15% of epoxy resin quality.
7. the preparation method of Graphene modified epoxy zinc rich primer according to claim 5, it is characterised in that: step (1) is heated with stirring to 80 DEG C, puts into phthalic anhydride, continue stirring, 80 DEG C of insulation reaction.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106590384A (en) * | 2016-12-07 | 2017-04-26 | 陕西宝塔山油漆股份有限公司 | Graphene-modified waterborne cold spraying zinc coating and preparation method thereof |
| CN106634438A (en) * | 2016-12-27 | 2017-05-10 | 苏州高通新材料科技有限公司 | Graphene modified solvent type epoxy zinc-rich coating as well as preparation method and application thereof |
| CN107011767A (en) * | 2017-04-22 | 2017-08-04 | 郑州格莱菲高铁新材料科技有限公司 | A kind of zinc alkene anticorrosive paint for railway facilities of permanent way and bridges steel construction workpiece |
| CN107828309A (en) * | 2017-11-02 | 2018-03-23 | 杭州烯创科技有限公司 | Dispersion that a kind of graphene anticorrosive paint uses and preparation method thereof |
| CN108285681A (en) * | 2017-03-13 | 2018-07-17 | 宁波市北仑区振古装饰设计研究院有限公司 | A kind of zinc powder incremental agent and its preparation method and application |
| CN108997893A (en) * | 2018-09-12 | 2018-12-14 | 浙江飞鲸新材料科技股份有限公司 | A kind of zinc-rich anti-corrosive paint and the preparation method and application thereof |
| CN109401532A (en) * | 2018-09-17 | 2019-03-01 | 中航百慕新材料技术工程股份有限公司 | Graphene powder zinc-rich paint and preparation method thereof |
| CN109486347A (en) * | 2018-11-05 | 2019-03-19 | 浙江山力得新材料科技有限公司 | A kind of anticorrosion coating material and preparation method thereof applied to para-seismic support |
| CN109486343A (en) * | 2018-09-17 | 2019-03-19 | 中航百慕新材料技术工程股份有限公司 | Graphene powder bimetallic coating and preparation method thereof |
| CN113563595A (en) * | 2021-07-14 | 2021-10-29 | 南方电网科学研究院有限责任公司 | Bentonite grafting agent and preparation method and application thereof |
| CN114133831A (en) * | 2021-12-28 | 2022-03-04 | 南昌航空大学 | Graphene oxide water-based epoxy coating and preparation method thereof |
| CN117363055A (en) * | 2023-10-16 | 2024-01-09 | 甘肃省交通规划勘察设计院股份有限公司 | Porphyrin modified graphene and preparation method and application thereof |
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| CN106590384B (en) * | 2016-12-07 | 2019-05-14 | 陕西宝塔山油漆股份有限公司 | A kind of aqueous syncretic zinc cold spray coating and preparation method thereof that graphene is modified |
| CN106590384A (en) * | 2016-12-07 | 2017-04-26 | 陕西宝塔山油漆股份有限公司 | Graphene-modified waterborne cold spraying zinc coating and preparation method thereof |
| CN106634438A (en) * | 2016-12-27 | 2017-05-10 | 苏州高通新材料科技有限公司 | Graphene modified solvent type epoxy zinc-rich coating as well as preparation method and application thereof |
| CN108285681A (en) * | 2017-03-13 | 2018-07-17 | 宁波市北仑区振古装饰设计研究院有限公司 | A kind of zinc powder incremental agent and its preparation method and application |
| CN107011767A (en) * | 2017-04-22 | 2017-08-04 | 郑州格莱菲高铁新材料科技有限公司 | A kind of zinc alkene anticorrosive paint for railway facilities of permanent way and bridges steel construction workpiece |
| CN107828309A (en) * | 2017-11-02 | 2018-03-23 | 杭州烯创科技有限公司 | Dispersion that a kind of graphene anticorrosive paint uses and preparation method thereof |
| CN107828309B (en) * | 2017-11-02 | 2020-03-31 | 杭州烯创科技有限公司 | Dispersion used for graphene anticorrosive paint and preparation method thereof |
| CN108997893A (en) * | 2018-09-12 | 2018-12-14 | 浙江飞鲸新材料科技股份有限公司 | A kind of zinc-rich anti-corrosive paint and the preparation method and application thereof |
| CN109401532A (en) * | 2018-09-17 | 2019-03-01 | 中航百慕新材料技术工程股份有限公司 | Graphene powder zinc-rich paint and preparation method thereof |
| CN109486343A (en) * | 2018-09-17 | 2019-03-19 | 中航百慕新材料技术工程股份有限公司 | Graphene powder bimetallic coating and preparation method thereof |
| CN109486347A (en) * | 2018-11-05 | 2019-03-19 | 浙江山力得新材料科技有限公司 | A kind of anticorrosion coating material and preparation method thereof applied to para-seismic support |
| CN113563595A (en) * | 2021-07-14 | 2021-10-29 | 南方电网科学研究院有限责任公司 | Bentonite grafting agent and preparation method and application thereof |
| CN113563595B (en) * | 2021-07-14 | 2023-06-06 | 南方电网科学研究院有限责任公司 | Bentonite grafting agent and preparation method and application thereof |
| CN114133831A (en) * | 2021-12-28 | 2022-03-04 | 南昌航空大学 | Graphene oxide water-based epoxy coating and preparation method thereof |
| CN117363055A (en) * | 2023-10-16 | 2024-01-09 | 甘肃省交通规划勘察设计院股份有限公司 | Porphyrin modified graphene and preparation method and application thereof |
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