CN107556882A - A kind of graphene antistatic coating and preparation method thereof - Google Patents

A kind of graphene antistatic coating and preparation method thereof Download PDF

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Publication number
CN107556882A
CN107556882A CN201710972747.7A CN201710972747A CN107556882A CN 107556882 A CN107556882 A CN 107556882A CN 201710972747 A CN201710972747 A CN 201710972747A CN 107556882 A CN107556882 A CN 107556882A
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added
antistatic
graphene
taken
stirs
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方万漂
周志强
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Wenzhou Win Innovation Material Technology Co Ltd
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Wenzhou Win Innovation Material Technology Co Ltd
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Abstract

The invention discloses a kind of graphene antistatic coating, and it is made up of the raw material of following weight parts:Glycerol monostearate monoesters 0.4 1, graphene 17 20, epoxy resin E44 110 130, dodecyldimethylammonium hydroxide inner salt 12,8 oxyquinolines 0.3 0.5, polyethylene glycol 56, antistatic emulsion 16 20, resorcinol 0.1 0.2, BFEE 0.07 0.1, borax 23, potassium permanganate 46, the present invention is also added into the graphene of oxidation, the antistatic emulsion is introduced in the oxidation preparation process of graphene, being effectively combined for graphene oxide and antistatic emulsion is realized, while also promotes the dispersiveness of graphene oxide in the epoxy.

Description

A kind of graphene antistatic coating and preparation method thereof
Technical field
The invention belongs to paint field, and in particular to a kind of graphene antistatic coating and preparation method thereof.
Background technology
Epoxy resin is used for coating maximum with liquid resin portion, but industrially using at present in anticorrosive coating Major part is solvent based coating, and conventional solution-type coating is more using aromatic hydrocarbons, esters, alcohols, ketone etc. as solvent, and these solvents are equal With different degrees of toxicity, and volatile matter is directly discharged into air, and environmental pollution is heavier.With the increasing of people's environmental consciousness By force, the novel anticorrosion coating such as green such as powdery paints, solventless coatings and water paint without organic solvent or low VOC Coating is developed in succession.Powdery paints is because condition of cure is more harsh, so as to limit its development;Solventless epoxy coating exists Solvent free paint field is that comparison is successful, simply in recent years reactive diluent hypotoxicity and curing agent it is safe and reliable Property etc. is challenged, among improving;And waterborne epoxy coatings is in addition to the plurality of advantages for adhering to solvent based coating, To improving performance, reducing pollution, expansion application etc. development, oneself covers locomotive, aviation, food, building etc. in its field, Therefore waterborne epoxy coatings is to develop a very rapid field in recent years;
Any object all carries the electrostatic charge of itself, and this electric charge can be that negative electrical charge can also be positive charge, and electrostatic charge is gathered Collection makes life or industrial production be affected or even endanger, and epoxy coating is mostly used for metal base at present, but it is anti- Static behaviour is poor, causes metal base product to cause unnecessary harm in use.
The content of the invention
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of graphene antistatic coating and its Preparation method.
To achieve the above object, the present invention uses following technical scheme:
A kind of graphene antistatic coating, it is made up of the raw material of following weight parts:
Glycerol monostearate monoesters 0.4-1, graphene 17-20, epoxy resin E44 110-130, dodecyl dimethyl beet Alkali 1-2,8-hydroxyquinoline 0.3-0.5, polyethylene glycol 5-6, antistatic emulsion 16-20, resorcinol 0.1-0.2, boron trifluoride Ether 0.07-0.1, borax 2-3, potassium permanganate 4-6.
What described antistatic emulsion was made up of the raw material of following weight parts:
Lauroyl both sexes base diethyl acid disodium 0.4-1, trihydroxy ethylamine oleate soap 2-4, basic zirconium phosphate 10-13, tetrahydrofurfuryl alcohol 0.1- 0.2nd, cellulose propionate 3-5, silane coupler kh550 0.7-1.
The preparation method of described antistatic emulsion comprises the following steps:
(1)Basic zirconium phosphate, trihydroxy ethylamine oleate soap mixing are taken, is added in the absolute ethyl alcohol of 24-30 times of compound weight, stirring is equal It is even, silane coupler kh550 is added, the insulated and stirred 1-2 hours at 60-65 DEG C, obtains silanol dispersion liquid;
(2)Cellulose propionate is taken, is added in the deionized water of 10-15 times of its weight, stirs, be added dropwise 0.5-1mol/l's Ammoniacal liquor, regulation pH are 10-12, are sent in 70-80 DEG C of water bath with thermostatic control, insulated and stirred 20-30 minutes, add lauroyl both sexes Base diethyl acid disodium, stirs, obtains fiber dispersion;
(3)Above-mentioned silanol dispersion liquid, fiber dispersion mixing are taken, tetrahydrofurfuryl alcohol is added, ultrasonic 10-20 minutes, obtains described anti- Electrostatic emulsion.
A kind of preparation method of black alkene antistatic coating, comprises the following steps:
(1)8-hydroxyquinoline is taken, is added in the absolute ethyl alcohol of 17-20 times of its weight, stirs, with above-mentioned antistatic emulsion Mixing, stirs, and adds glycerol monostearate monoesters, the insulated and stirred 4-10 minutes at 60-70 DEG C, obtains antistatic Composite Milk Liquid;
(2)Dodecyldimethylammonium hydroxide inner salt is taken, is added in the deionized water of 20-30 times of its weight, stirs, adds boron Sand, ultrasonic 4-5 minutes, obtain aqueous dispersions;
(3)Above-mentioned antistatic complex emulsions, aqueous dispersions mixing are taken, stirs, obtains premixed solution;
(4)Graphene is taken, in sulfuric acid solution that be added to 15-20 times of its weight, 95-97%, stirring reaction 30-40 minutes, mistake Filter, precipitation to be washed, air drying, mixes, is added in above-mentioned premixed solution with potassium permanganate, rise temperature is 50-60 DEG C, Insulated and stirred 4-5 hours, obtain oxidation antistatic solution;
(5)Extracting epoxy resin E44, it is added in the deionized water of 30-40 times of its weight, stirs, adds above-mentioned oxidation and resist Electrostatic solution, BFEE, stir, and are sent in reactor, are passed through nitrogen, and regulation temperature of reaction kettle is 65-70 DEG C, insulated and stirred 2-3 hours, obtain water-base epoxy solution;
(6)Resorcinol is taken, is added in above-mentioned water-base epoxy solution, ultrasonic 30-40 minutes, ethanol is distilled off, with residue Each raw material mixing, 1600-2000 revs/min of stirring 1-2 hour, produces the graphene antistatic coating.
Advantages of the present invention:
Using lauroyl both sexes base diethyl acid disodium as antistatic additive in the antistatic emulsion that the present invention adds, basic zirconium phosphate, propionic acid are fine Dimension element can then improve the toughness and mechanical strength of finished product coating, and the present invention is silane-modified by basic zirconium phosphate, cellulose propionate progress, Its scattered compatibility in the epoxy is effectively raised, improves the uniform and stable property of finished product film, the present invention also adds Entered oxidation graphene, the antistatic emulsion is introduced in the oxidation preparation process of graphene, realize graphene oxide with Antistatic emulsion is effectively combined, while also promotes the dispersiveness of graphene oxide in the epoxy.
Embodiment
Embodiment 1
A kind of graphene antistatic coating, it is made up of the raw material of following weight parts:
Glycerol monostearate monoesters 1, graphene 20, epoxy resin E44 130, dodecyldimethylammonium hydroxide inner salt 2,8- hydroxyl quinolines Quinoline 0.5, polyethylene glycol 6, antistatic emulsion 20, resorcinol 0.2, BFEE 0.1, borax 3, potassium permanganate 6.
What described antistatic emulsion was made up of the raw material of following weight parts:
Lauroyl both sexes base diethyl acid disodium 1, trihydroxy ethylamine oleate soap 4, basic zirconium phosphate 13, tetrahydrofurfuryl alcohol 0.2, cellulose propionate 5, Silane coupler kh550 1.
The preparation method of described antistatic emulsion comprises the following steps:
(1)Basic zirconium phosphate, trihydroxy ethylamine oleate soap mixing are taken, is added in the absolute ethyl alcohol of 30 times of compound weight, stirs, Silane coupler kh550 is added, insulated and stirred 2 hours at 65 DEG C, obtains silanol dispersion liquid;
(2)Cellulose propionate is taken, is added in the deionized water of 15 times of its weight, stirs, 1mol/l ammoniacal liquor is added dropwise, is adjusted It is 12 to save pH, is sent in 80 DEG C of water bath with thermostatic control, insulated and stirred 30 minutes, adds lauroyl both sexes base diethyl acid disodium, stirs Mix uniformly, obtain fiber dispersion;
(3)Above-mentioned silanol dispersion liquid, fiber dispersion mixing are taken, tetrahydrofurfuryl alcohol is added, ultrasound 20 minutes, obtains described antistatic Emulsion.
A kind of preparation method of graphene antistatic coating, comprises the following steps:
(1)8-hydroxyquinoline is taken, is added in the absolute ethyl alcohol of 20 times of its weight, stirs, is mixed with above-mentioned antistatic emulsion Close, stir, add glycerol monostearate monoesters, insulated and stirred 10 minutes at 70 DEG C, obtain antistatic complex emulsions;
(2)Dodecyldimethylammonium hydroxide inner salt is taken, is added in the deionized water of 30 times of its weight, stirs, adds borax, Ultrasound 5 minutes, obtains aqueous dispersions;
(3)Above-mentioned antistatic complex emulsions, aqueous dispersions mixing are taken, stirs, obtains premixed solution;
(4)Graphene is taken, is added in 20 times of its weight, 97% sulfuric acid solution, stirring reaction 40 minutes, filtering, will be precipitated Washing, air drying, mixes with potassium permanganate, is added in above-mentioned premixed solution, and rise temperature is 60 DEG C, and insulated and stirred 5 is small When, obtain oxidation antistatic solution;
(5)Extracting epoxy resin E44, it is added in the deionized water of 40 times of its weight, stirs, it is antistatic to add above-mentioned oxidation Solution, BFEE, stir, and are sent in reactor, are passed through nitrogen, and regulation temperature of reaction kettle is 70 DEG C, insulation Stirring 3 hours, obtains water-base epoxy solution;
(6)Resorcinol is taken, is added in above-mentioned water-base epoxy solution, ultrasound 40 minutes, ethanol is distilled off, with remaining each original Material mixing, 2000 revs/min are stirred 2 hours, produce the graphene antistatic coating.
Embodiment 2
A kind of graphene antistatic coating, it is made up of the raw material of following weight parts:
Glycerol monostearate monoesters 0.4, graphene 17, epoxy resin E44 110, dodecyldimethylammonium hydroxide inner salt 1,8- hydroxyls Quinoline 0.3, polyethylene glycol 5, antistatic emulsion 16, resorcinol 0.1, BFEE 0.07, borax 2, potassium permanganate 4.
What described antistatic emulsion was made up of the raw material of following weight parts:
Lauroyl both sexes base diethyl acid disodium 0.4, trihydroxy ethylamine oleate soap 2, basic zirconium phosphate 10, tetrahydrofurfuryl alcohol 0.1, cellulose propionate 3rd, silane coupler kh550 0.7.
The preparation method of described antistatic emulsion comprises the following steps:
(1)Basic zirconium phosphate, trihydroxy ethylamine oleate soap mixing are taken, is added in the absolute ethyl alcohol of 24 times of compound weight, stirs, Silane coupler kh550 is added, insulated and stirred 1 hour at 60 DEG C, obtains silanol dispersion liquid;
(2)Cellulose propionate is taken, is added in the deionized water of 10 times of its weight, stirs, 0.5mol/l ammoniacal liquor is added dropwise, It is 10 to adjust pH, is sent in 70 DEG C of water bath with thermostatic control, insulated and stirred 20 minutes, adds lauroyl both sexes base diethyl acid disodium, Stir, obtain fiber dispersion;
(3)Above-mentioned silanol dispersion liquid, fiber dispersion mixing are taken, tetrahydrofurfuryl alcohol is added, ultrasound 10 minutes, obtains described antistatic Emulsion.
A kind of preparation method of graphene antistatic coating, comprises the following steps:
(1)8-hydroxyquinoline is taken, is added in the absolute ethyl alcohol of 17 times of its weight, stirs, is mixed with above-mentioned antistatic emulsion Close, stir, add glycerol monostearate monoesters, insulated and stirred 4 minutes at 60 DEG C, obtain antistatic complex emulsions;
(2)Dodecyldimethylammonium hydroxide inner salt is taken, is added in the deionized water of 20 times of its weight, stirs, adds borax, Ultrasonic 4-5 minutes, obtain aqueous dispersions;
(3)Above-mentioned antistatic complex emulsions, aqueous dispersions mixing are taken, stirs, obtains premixed solution;
(4)Graphene is taken, is added in 15 times of its weight, 95% sulfuric acid solution, stirring reaction 30 minutes, filtering, will be precipitated Washing, air drying, mixes with potassium permanganate, is added in above-mentioned premixed solution, and rise temperature is 50 DEG C, and insulated and stirred 4 is small When, obtain oxidation antistatic solution;
(5)Extracting epoxy resin E44, it is added in the deionized water of 30 times of its weight, stirs, it is antistatic to add above-mentioned oxidation Solution, BFEE, stir, and are sent in reactor, are passed through nitrogen, and regulation temperature of reaction kettle is 65 DEG C, insulation Stirring 2 hours, obtains water-base epoxy solution;
(6)Resorcinol is taken, is added in above-mentioned water-base epoxy solution, ultrasound 30 minutes, ethanol is distilled off, with remaining each original Material mixing, 16000 revs/min are stirred 1 hour, produce the graphene antistatic coating.
Performance test:
By the graphene antistatic coating of the embodiment of the present invention 1, the graphene antistatic coating of embodiment 2, Commercial epoxy coating It is respectively coated in identical metallic substrate surface, it is respectively 10 to measure sheet resistance10Ω、109Ω、105Ω;As can be seen that this The antistatic coating of invention has more preferable antistatic effect.

Claims (4)

1. a kind of graphene antistatic coating, it is characterised in that it is made up of the raw material of following weight parts:
Glycerol monostearate monoesters 0.4-1, graphene 17-20, epoxy resin E44 110-130, dodecyl dimethyl beet Alkali 1-2,8-hydroxyquinoline 0.3-0.5, polyethylene glycol 5-6, antistatic emulsion 16-20, resorcinol 0.1-0.2, boron trifluoride Ether 0.07-0.1, borax 2-3, potassium permanganate 4-6.
A kind of 2. graphene antistatic coating according to claim 1, it is characterised in that described antistatic emulsion be by The raw material composition of following weight parts:
Lauroyl both sexes base diethyl acid disodium 0.4-1, trihydroxy ethylamine oleate soap 2-4, basic zirconium phosphate 10-13, tetrahydrofurfuryl alcohol 0.1- 0.2nd, cellulose propionate 3-5, silane coupler kh550 0.7-1.
A kind of 3. graphene antistatic coating according to claim 2, it is characterised in that the system of described antistatic emulsion Preparation Method comprises the following steps:
(1)Basic zirconium phosphate, trihydroxy ethylamine oleate soap mixing are taken, is added in the absolute ethyl alcohol of 24-30 times of compound weight, stirring is equal It is even, silane coupler kh550 is added, the insulated and stirred 1-2 hours at 60-65 DEG C, obtains silanol dispersion liquid;
(2)Cellulose propionate is taken, is added in the deionized water of 10-15 times of its weight, stirs, be added dropwise 0.5-1mol/l's Ammoniacal liquor, regulation pH are 10-12, are sent in 70-80 DEG C of water bath with thermostatic control, insulated and stirred 20-30 minutes, add lauroyl both sexes Base diethyl acid disodium, stirs, obtains fiber dispersion;
(3)Above-mentioned silanol dispersion liquid, fiber dispersion mixing are taken, tetrahydrofurfuryl alcohol is added, ultrasonic 10-20 minutes, obtains described anti- Electrostatic emulsion.
4. a kind of preparation method of graphene antistatic coating as claimed in claim 1, it is characterised in that including following step Suddenly:
(1)8-hydroxyquinoline is taken, is added in the absolute ethyl alcohol of 17-20 times of its weight, stirs, with above-mentioned antistatic emulsion Mixing, stirs, and adds glycerol monostearate monoesters, the insulated and stirred 4-10 minutes at 60-70 DEG C, obtains antistatic Composite Milk Liquid;
(2)Dodecyldimethylammonium hydroxide inner salt is taken, is added in the deionized water of 20-30 times of its weight, stirs, adds boron Sand, ultrasonic 4-5 minutes, obtain aqueous dispersions;
(3)Above-mentioned antistatic complex emulsions, aqueous dispersions mixing are taken, stirs, obtains premixed solution;
(4)Graphene is taken, in sulfuric acid solution that be added to 15-20 times of its weight, 95-97%, stirring reaction 30-40 minutes, mistake Filter, precipitation to be washed, air drying, mixes, is added in above-mentioned premixed solution with potassium permanganate, rise temperature is 50-60 DEG C, Insulated and stirred 4-5 hours, obtain oxidation antistatic solution;
(5)Extracting epoxy resin E44, it is added in the deionized water of 30-40 times of its weight, stirs, adds above-mentioned oxidation and resist Electrostatic solution, BFEE, stir, and are sent in reactor, are passed through nitrogen, and regulation temperature of reaction kettle is 65-70 DEG C, insulated and stirred 2-3 hours, obtain water-base epoxy solution;
(6)Resorcinol is taken, is added in above-mentioned water-base epoxy solution, ultrasonic 30-40 minutes, ethanol is distilled off, with residue Each raw material mixing, 1600-2000 revs/min of stirring 1-2 hour, produces the graphene antistatic coating.
CN201710972747.7A 2017-10-18 2017-10-18 A kind of graphene antistatic coating and preparation method thereof Pending CN107556882A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108276712A (en) * 2018-01-30 2018-07-13 温州市赢创新材料技术有限公司 A kind of antistatic cross-linked graphene film and preparation method thereof
CN109266169A (en) * 2018-09-07 2019-01-25 汪青霞 A kind of antistatic metallic paint and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106244011A (en) * 2016-08-02 2016-12-21 江苏晨光涂料有限公司 Graphene-based aqueous antistatic coating and preparation method thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106244011A (en) * 2016-08-02 2016-12-21 江苏晨光涂料有限公司 Graphene-based aqueous antistatic coating and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108276712A (en) * 2018-01-30 2018-07-13 温州市赢创新材料技术有限公司 A kind of antistatic cross-linked graphene film and preparation method thereof
CN109266169A (en) * 2018-09-07 2019-01-25 汪青霞 A kind of antistatic metallic paint and preparation method thereof

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