CN106189455A - A kind of preparation method of the fire-retardant corrosion resistant coating comprising modified graphene - Google Patents

A kind of preparation method of the fire-retardant corrosion resistant coating comprising modified graphene Download PDF

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Publication number
CN106189455A
CN106189455A CN201610570515.4A CN201610570515A CN106189455A CN 106189455 A CN106189455 A CN 106189455A CN 201610570515 A CN201610570515 A CN 201610570515A CN 106189455 A CN106189455 A CN 106189455A
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preparation
houghite
graphene
solution
coating
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张哲夫
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/18—Fireproof paints including high temperature resistant paints
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/40—Compounds of aluminium
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/08—Anti-corrosive paints
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/08—Anti-corrosive paints
    • C09D5/10—Anti-corrosive paints containing metal dust
    • C09D5/103—Anti-corrosive paints containing metal dust containing Al
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/08—Anti-corrosive paints
    • C09D5/10—Anti-corrosive paints containing metal dust
    • C09D5/106—Anti-corrosive paints containing metal dust containing Zn

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Inorganic Chemistry (AREA)
  • Paints Or Removers (AREA)

Abstract

The present invention relates to the preparation method of a kind of fire-retardant corrosion resistant coating comprising modified graphene, have employed stratiform houghite and modified graphene coordinates being modified of intercalator, it is prepared for the coating of a kind of high corrosion-resistant, add modified graphene and can promote the inorganic coating adhesive force to metal, improve its interface property, not only for thicker coating, there is preferably antiseptic property, still can keep the anti-corrosive properties of its excellence for relatively thin coating.

Description

A kind of preparation method of the fire-retardant corrosion resistant coating comprising modified graphene
Technical field
The present invention relates to the preparation method of a kind of fire-retardant corrosion resistant coating comprising modified graphene, belong to construction material neck Territory.
Background technology
Anticorrosive paint is a kind of priming paint being provided that cathodic protection, is commonly used to industrial equipment.Steel substrate can be protected, Reducing the risk of corrosion, this coating is with the weatherability of its excellence, solvent resistance, outstanding anticorrosive property and selfreparing merit Can, in the heavy antisepsis fields such as railroad bridge, port and pier, shipping container, obtained large-scale application.
Study general uses inorganic non-metallic corrosion inhibiter or is mixed into additive to replace part zinc particles to improve at present The corrosion resistance of coating, or change zinc particles pattern study it to coating corrupting influence.Additionally, the thickness pair of coating Antiseptic property also has large effect, if in general coating is relatively thin, and the formation crack of zinc oxide, near zinc oxide, add The infiltration of speed electrolyte, is therefore unfavorable for anticorrosion.The most current coating yet suffers from the shortcoming that flame-proof heat-resistant performance is the strongest.
Determine it owing to modified graphene has preferable one-dimentional structure there is special character, the most excellent mechanics, The character such as electricity, calorifics so that it is before material science, chemistry, physics etc. hand over justice ambit to show wide application Scape, adds modified graphene and is modified having broad application prospects to coating.
Summary of the invention
The many deficiencies existed for existing coating, the invention provides and a kind of comprise the fire-retardant corrosion-resistant of modified graphene The preparation method of coating, concrete preparation process includes:
(1) by ZnCl2、FeCl3And FeCl2It is dissolved into respectively in water, is configured to the solution that concentration is 1～2mol/L, molten by three kinds Liquid mixes, and keeps Zn2+: Fe2+: Fe3+Mol ratio be (3～5): (2～3): 1, instill certain in constant temperature 60～80 DEG C of water-baths The alkaline solution of amount, reacts 2～3h, forms the houghite precipitation with layer structure；
(2) graphene oxide is soluble in water, ultrasonic disperse, obtain graphene oxide dispersion, regulate dispersion liquid pH with acetic acid Value is 3-5, adds ethylenediamine, stirs, and reaction terminates rear deionized water wash, filtration；Then by filter cake dispersion with go from In the solvent of son and ethanol, addition sodium borohydride, 60-80 DEG C, back flow reaction 4-10 hour, filters, obtains ethylenediamine modification stone Ink alkene；
(3) 6 mass parts houghite precipitations step (1) prepared add the ethylenediamine modified graphene 2 that step (2) obtains Mass parts, intercalator 1 mass parts, and after being placed in the reactor of politef, put in baking oven, at 70-90 DEG C It is incubated 8-24h, after naturally cooling to room temperature, centrifugal filtration, washing under the conditions of stationary temperature, dries, obtain Graphene modified Houghite precipitates；
(4) Graphene modification houghite precipitation step (3) prepared joins in deionized water and alcohol mixeding liquid, adjusts PH value is to 6.5 ~ 7.5, at room temperature, stirs 2 ~ 4h, then 20 ~ 50g aluminum zinc powder or zinc-aluminium solution is at room temperature joined Stating in solution, stir 0.5 ~ 2h, products therefrom centrifuge separates, and uses washing with alcohol, in an oven 40 ~ 60 DEG C of drying, i.e. Obtain fire-retardant corrosion resistant coating.
Wherein, described intercalator is cetyl trimethylammonium bromide, hexadecyltrimethylammonium chloride, diallyl two Any one of ammonio methacrylate.
Wherein, in step (2), the mass ratio of graphene oxide and ethylenediamine is 1:6-12.
Wherein, described zinc-aluminium solution is zinc phosphate or aluminum phosphate solution.
Beneficial effects of the present invention:
Coating is studied by the present invention at the antiseptic property of cold rolling steel matrix, have employed stratiform houghite and modified stone Ink alkene coordinates being modified of intercalator, is prepared for the coating of a kind of high corrosion-resistant, adds modified graphene and can promote inorganic The coating adhesive force to metal, improves its interface property, has preferably antiseptic property not only for thicker coating, for Relatively thin coating still can keep the anti-corrosive properties of its excellence.
By Graphene is carried out partially modified, introduce organo-functional group, the stability of graphene-structured can be conducive to, Join in coating, improve the aging resistance of coating, resistance to elevated temperatures, play efficient fire-retardant purpose.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is further detailed explanation.
Embodiment 1
(1) by ZnCl2、FeCl3And FeCl2It is dissolved into respectively in water, is configured to the solution that concentration is 1mol/L, by three kinds of solution Mixing, keeps Zn2+: Fe2+: Fe3+Mol ratio be 3:2:1, in 60 DEG C of water-baths of constant temperature, instill a certain amount of alkaline solution, instead Answer 2h, form the houghite precipitation with layer structure；
(2) graphene oxide is soluble in water, ultrasonic disperse, obtain graphene oxide dispersion, regulate dispersion liquid pH with acetic acid Value is 3, adds ethylenediamine, stirs, and reaction terminates rear deionized water wash, filtration；Then by filter cake dispersion and deionization With in the solvent of ethanol, add sodium borohydride, 60 DEG C, back flow reaction 4 hours, filter, obtain ethylenediamine modified graphene；
(3) 6 mass parts houghite precipitations step (1) prepared add the ethylenediamine modified graphene 2 that step (2) obtains Mass parts, for cetyl trimethylammonium bromide 1 mass parts, and after being placed in the reactor of politef, put into In baking oven, under the conditions of 70 DEG C of stationary temperatures, it is incubated 8h, after naturally cooling to room temperature, centrifugal filtration, washing, dries, obtain Graphene modification houghite precipitates；
(4) Graphene modification houghite precipitation step (3) prepared joins in deionized water and alcohol mixeding liquid, adjusts PH value is to 6.5, at room temperature, stirs 2h, then at room temperature joins in above-mentioned solution by 20g aluminum zinc powder, stirs 0.5h, institute Obtaining product centrifuge to separate, use washing with alcohol, 40 DEG C of drying, obtain fire-retardant corrosion resistant coating in an oven.
Embodiment 2
(1) by ZnCl2、FeCl3And FeCl2It is dissolved into respectively in water, is configured to the solution that concentration is 2mol/L, by three kinds of solution Mixing, keeps Zn2+: Fe2+: Fe3+Mol ratio be 5:3:1, in 80 DEG C of water-baths of constant temperature, instill a certain amount of alkaline solution, instead Answer 3h, form the houghite precipitation with layer structure；
(2) graphene oxide is soluble in water, ultrasonic disperse, obtain graphene oxide dispersion, regulate dispersion liquid pH with acetic acid Value is 5, adds ethylenediamine, stirs, and reaction terminates rear deionized water wash, filtration；Then by filter cake dispersion and deionization With in the solvent of ethanol, add sodium borohydride, 80 DEG C, back flow reaction 10 hours, filter, obtain ethylenediamine modified graphene；
(3) 6 mass parts houghite precipitations step (1) prepared add the ethylenediamine modified graphene 2 that step (2) obtains Mass parts, hexadecyltrimethylammonium chloride 1 mass parts, and after being placed in the reactor of politef, put into baking In case, under the conditions of 90 DEG C of stationary temperatures, it is incubated 24h, after naturally cooling to room temperature, centrifugal filtration, washing, dries, obtain stone Ink alkene modification houghite precipitation；
(4) Graphene modification houghite precipitation step (3) prepared joins in deionized water and alcohol mixeding liquid, adjusts PH value is to 7.5, at room temperature, stirs 4h, then at room temperature joins in above-mentioned solution by 50g aluminum zinc powder, stirs 2h, gained Product centrifuge separates, and uses washing with alcohol, and 60 DEG C of drying, obtain fire-retardant corrosion resistant coating in an oven.
Embodiment 3
(1) by ZnCl2、FeCl3And FeCl2It is dissolved into respectively in water, is configured to the solution that concentration is 1.5mol/L, molten by three kinds Liquid mixes, and keeps Zn2+: Fe2+: Fe3+Mol ratio be 4:3:1, in 70 DEG C of water-baths of constant temperature, instill a certain amount of alkaline solution, Reaction 3h, forms the houghite precipitation with layer structure；
(2) graphene oxide is soluble in water, ultrasonic disperse, obtain graphene oxide dispersion, regulate dispersion liquid pH with acetic acid Value is 4, adds ethylenediamine, stirs, and reaction terminates rear deionized water wash, filtration；Then by filter cake dispersion and deionization With in the solvent of ethanol, add sodium borohydride, 70 DEG C, back flow reaction 6 hours, filter, obtain ethylenediamine modified graphene；
(3) 6 mass parts houghite precipitations step (1) prepared add the ethylenediamine modified graphene 2 that step (2) obtains Mass parts, diallyldimethylammonium chloride 1 mass parts, and after being placed in the reactor of politef, put into baking In case, under the conditions of 80 DEG C of stationary temperatures, it is incubated 16h, after naturally cooling to room temperature, centrifugal filtration, washing, dries, obtain stone Ink alkene modification houghite precipitation；
(4) Graphene modification houghite precipitation step (3) prepared joins in deionized water and alcohol mixeding liquid, adjusts PH value is to 7, at room temperature, stirs 3h, then at room temperature joins in above-mentioned solution by 30g zinc-aluminium solution, stirs 1h, gained Product centrifuge separates, and uses washing with alcohol, and 50 DEG C of drying, obtain fire-retardant corrosion resistant coating in an oven.
Comparative example 1
Not being modified Graphene, other experiment parameters are with embodiment 1.
Comparative example 2
Being added without modified graphene, other experiment parameters are with embodiment 1.
Concrete detection
Concrete outcome is shown in Table 1.
Each Testing index of coating
Embodiment 1 Embodiment 2 Embodiment 3 Comparative example 1 Comparative example 2 Examination criteria
Adhesive force 1 grade 1 grade 1 grade 2 grades 2 grades GB/T9286-1998
Hardness H H H HB HB GB/T1723-1993
Viscosity (cps) 23 24 23 24 24 GB/T1732-1993
Impact resistance (kg x cm) 65 68 66 40 35 GB/T9264-2012
Salt fog resistance (h) 275 288 285 200 181 GB/T1771-1991
There is the above results it can be seen that modified graphene advantageously reduces the density of coating, significantly improve the anti-flammability of coating, resistance to Corrosive nature.
The above, the only detailed description of the invention of the present invention, but protection scope of the present invention is not limited thereto, and any Those of ordinary skill in the art in the technical scope that disclosed herein, the change that can expect without creative work or Replace, all should contain within protection scope of the present invention.Therefore, protection scope of the present invention should be limited with claims Fixed protection domain is as the criterion.

Claims (5)

1. the preparation method of the fire-retardant corrosion resistant coating comprising modified graphene, it is characterised in that concrete preparation process bag Include:
(1) by ZnCl2、FeCl3And FeCl2It is dissolved into respectively in water, is configured to the solution that concentration is 1～2mol/L, molten by three kinds Liquid mixes, and keeps Zn2+: Fe2+: Fe3+Mol ratio be (3～5): (2～3): 1, instill certain in constant temperature 60～80 DEG C of water-baths The alkaline solution of amount, reacts 2～3h, forms the houghite precipitation with layer structure；
(2) graphene oxide is soluble in water, ultrasonic disperse, obtain graphene oxide dispersion, regulate dispersion liquid pH with acetic acid Value is 3-5, adds ethylenediamine, stirs, and reaction terminates rear deionized water wash, filtration；Then by filter cake dispersion with go from In the solvent of son and ethanol, addition sodium borohydride, 60-80 DEG C, back flow reaction 4-10 hour, filters, obtains ethylenediamine modification stone Ink alkene；
(3) 6 mass parts houghite precipitations step (1) prepared add the ethylenediamine modified graphene 2 that step (2) obtains Mass parts, intercalator 1 mass parts, and after being placed in the reactor of politef, put in baking oven, at 70-90 DEG C It is incubated 8-24h, after naturally cooling to room temperature, centrifugal filtration, washing under the conditions of stationary temperature, dries, obtain Graphene modified Houghite precipitates；
(4) Graphene modification houghite precipitation step (3) prepared joins in deionized water and alcohol mixeding liquid, adjusts PH value is to 6.5 ~ 7.5, at room temperature, stirs 2 ~ 4h, then 20 ~ 50g aluminum zinc powder or zinc-aluminium solution is at room temperature joined Stating in solution, stir 0.5 ~ 2h, products therefrom centrifuge separates, and uses washing with alcohol, in an oven 40 ~ 60 DEG C of drying, i.e. Obtain fire-retardant corrosion resistant coating.
2. preparation method as claimed in claim 1, it is characterised in that described intercalator be cetyl trimethylammonium bromide, Any one of hexadecyltrimethylammonium chloride, diallyldimethylammonium chloride etc..
3. preparation method as claimed in claim 1, it is characterised in that graphene oxide and the quality of ethylenediamine in step (2) Ratio is 1:6-12.
4. preparation method as claimed in claim 1, it is characterised in that layered houghite is Kaolin, Vermiculitum, Muscovitum In Deng one or more.
5. preparation method as claimed in claim 1, it is characterised in that described zinc-aluminium solution is zinc phosphate or aluminum phosphate solution.
CN201610570515.4A 2016-07-20 2016-07-20 A kind of preparation method of the fire-retardant corrosion resistant coating comprising modified graphene Pending CN106189455A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106995643A (en) * 2017-05-23 2017-08-01 上海工程技术大学 A kind of water paint of graphene-containing/zinc-aluminum gavite nano-complex and preparation method thereof
CN113462268A (en) * 2021-07-14 2021-10-01 苏州嘉乐威新材料股份有限公司 Environment-friendly varnish for corrosion prevention of petroleum pipeline and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102757097A (en) * 2012-02-22 2012-10-31 太原理工大学 Method for rapidly preparing nanocrystalline zinc-iron hydrotalcite
CN103805046A (en) * 2014-01-26 2014-05-21 陕西科技大学 Graphene-containing waterborne polyurethane composite conductive coating prepared in situ and preparation method thereof
CN105017965A (en) * 2015-08-21 2015-11-04 朱蕾 Preparation method of carbon nanotube-montmorillonite-silicone modified zinc-rich paint with corrosion resistance

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102757097A (en) * 2012-02-22 2012-10-31 太原理工大学 Method for rapidly preparing nanocrystalline zinc-iron hydrotalcite
CN103805046A (en) * 2014-01-26 2014-05-21 陕西科技大学 Graphene-containing waterborne polyurethane composite conductive coating prepared in situ and preparation method thereof
CN105017965A (en) * 2015-08-21 2015-11-04 朱蕾 Preparation method of carbon nanotube-montmorillonite-silicone modified zinc-rich paint with corrosion resistance

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106995643A (en) * 2017-05-23 2017-08-01 上海工程技术大学 A kind of water paint of graphene-containing/zinc-aluminum gavite nano-complex and preparation method thereof
CN106995643B (en) * 2017-05-23 2019-05-21 上海工程技术大学 A kind of water paint and preparation method thereof of containing graphene/zinc-aluminum gavite nano-complex
CN113462268A (en) * 2021-07-14 2021-10-01 苏州嘉乐威新材料股份有限公司 Environment-friendly varnish for corrosion prevention of petroleum pipeline and preparation method thereof

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