CN110484100A - A kind of antistatic coating and preparation method thereof - Google Patents
A kind of antistatic coating and preparation method thereof Download PDFInfo
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- CN110484100A CN110484100A CN201910665171.9A CN201910665171A CN110484100A CN 110484100 A CN110484100 A CN 110484100A CN 201910665171 A CN201910665171 A CN 201910665171A CN 110484100 A CN110484100 A CN 110484100A
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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
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
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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
- C09D125/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Coating compositions based on derivatives of such polymers
- C09D125/18—Homopolymers or copolymers of aromatic monomers containing elements other than carbon and hydrogen
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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
- C09D165/00—Coating compositions based on macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain; Coating compositions based on derivatives of such polymers
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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
- C09D5/24—Electrically-conducting paints
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/04—Antistatic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
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Abstract
The present invention provides a kind of antistatic coatings and preparation method thereof, PEDOT:PSS dispersion liquid, the tetraalkoxy compound of 1-20%, the silane coupling agent of 0.01-2%, the alcohols solvent of 5-50%, the high boiling solvent of 2-5%, the surfactant of 0.01-1%, the catalyst of 0.001-1% and the deionized water of 5-80% including 5-50%, belong to antistatic coating correlative technology field；By the present invention in that using silane coupling agent prehydrolysis as the presoma of tetraalkoxy compound hydrolysis, use tetraalkoxy compound hydrolysis as the mode of inorganic bond, hybrid inorganic-organic system is formed with PEDOT:PSS, preparation is the transparent antistatic coating of antistatic material of main part with PEDOT:PSS.Antistatic coating provided by the present invention is coated on substrate surface, obtains having both the antistatic coating of high-hardness, wearable and low square resistance by heat cure；Meanwhile antistatic coating of the invention also has antireflective effect.
Description
[technical field]
The invention belongs to antistatic coating correlative technology fields, and in particular to a kind of antistatic coating and preparation method thereof.
[background technique]
Existing permanent transparent anti-static material mainly has conducting polymer and metallic oxide type anti-static material, due to
Metal oxide generally needs to form a film using vapor deposition mode, and processing is cumbersome, cost is excessively high, and with poly- (3,4- ethylene dioxy thiophenes
Pheno)/poly- (styrene sulfonic acid), referred to as (PEDOT/PSS) is the conducting polymer of model in antistatic field Successful commercial
Change application.
But in the existing transparent antistatic coating based on PEDOT:PSS, however it remains hardness is low or the high problem of resistance value, such as
Chinese invention patent: a kind of active anti-static agents and its ultraviolet photocurable anti-static paint (publication number CN103627240A) lead to
Crossing the preparation of imidazoline intermediate, the introducing of active group and imidazoline intermediate quaternization step, to have obtained a kind of activity anti-
Electrostatic agent, the coating of available 1.0 × 10^8 of sheet resistance Ω/, hardness 2H；A kind of Chinese invention patent: antistatic UV hardening
Liquid (publication number CN108948393A), using acrylic monomers and initiator as UV film-forming object, hardness is up to 6H,
But sheet resistance is higher, reaches 1.0 × 10^6 Ω/.
In the above-mentioned transparent antistatic coating patents based on PEDOT:PSS, using organic bond as with PEDOT/PSS
Composite material, antistatic coating is widely used in the polymeric substrates such as acrylic, PET, PE.But due to generally existing hardness
Low disadvantage is unable to satisfy antistatic glass for the rigors of hardness and reliability.
[summary of the invention]
For the above-mentioned technical problems in the prior art, the present invention provides a kind of antistatic coating and its preparation sides
Method, the presoma by using silane coupling agent prehydrolysis as tetraalkoxy compound hydrolysis, uses tetraalkoxy compound
The mode as inorganic bond is hydrolyzed, forms hybrid inorganic-organic system with PEDOT:PSS, preparation is anti-with PEDOT:PSS
The transparent antistatic coating of dielectric body material.The antistatic coating, which is coated on substrate, can form the anti-of hard high-wearing feature
Electrostatic coating (hardness is up to 9H), and sheet resistance is low (up to 1.1 × 10^4 Ω/), it is to achieve the goals above, of the invention
Technical solution is as follows:
A kind of antistatic coating, by mass percentage, including following components:
The PEDOT:PSS dispersion liquid is poly- (3,4- ethene dioxythiophene): the aqueous dispersion of poly- (styrene sulfonate).
Preferably, the tetraalkoxy compound is positive quanmethyl silicate, tetraethyl orthosilicate, positive silicic acid orthocarbonate and silicon
One of or two or more mixture in sour four butyl esters.
Preferably, the silane coupling agent is 3- glycidyl ether oxygen propyl trimethoxy silicane, γ-methacryloxypropyl
Base propyl trimethoxy silicane, γ-mercaptopropyl trimethoxysilane, gamma-amino propyl trimethoxy silicane, gamma-amino propyl
It is triethoxysilane, vinyltrimethoxysilane, one of or two or more mixed in vinyltriethoxysilane
Close object.
Preferably, the alcohols solvent be methanol, ethyl alcohol, trifluoroethanol, isopropanol, isobutanol, n-amyl alcohol, sec-amyl alcohol,
One of or two or more mixture in diacetone alcohol.
Preferably, the high boiling solvent be dimethyl sulfoxide, ethylene glycol, propylene glycol, diethylene glycol (DEG), glycerine, formamide,
One of or two or more mixture in n,N-Dimethylformamide.
Preferably, the surfactant is alkyl phenol polyoxyethylene ether class ionic surface active agent, acetylenic diols surface
One of or two or more mixture in activating agent and fluorine carbon nonionic surfactant.
Preferably, the catalyst be formic acid, acetic acid, hydrochloric acid, nitric acid, sulfuric acid, the one of which in oxalic acid or two kinds with
On mixture.
The invention also discloses the preparation methods of above-mentioned antistatic coating, comprising the following steps:
S1: PEDOT:PSS dispersion liquid is added to the container, and sequentially adds deionized water, high boiling solvent, table while stirring
Face activating agent, alcohols solvent, silane coupling agent, stir evenly, and pre-hydrolyzed solution is made；
S2: pre-hydrolyzed solution is added in isothermal reaction container, and tetraalkoxy compound is added, is warming up to 60-100 DEG C, side
The side dropwise addition catalyst is stirred, after then sealing simultaneously insulated and stirred 10-20h, stopping is stirred and cooling, obtains antistatic painting
Material.
Compared to the prior art, beneficial effects of the present invention are as follows:
The present invention carries out prehydrolysis with silane coupling agent and forms presoma, so using PEDOT:PSS dispersion liquid as conductive component
It is heated after tetraalkoxy compound is added afterwards, hydrolyzes to form organic silicon sol, i.e. antistatic coating under the catalysis of the catalyst.
Silane coupling agent hydrolysate is wet silantriol RSi (OH)3, alkoxy R base is crosslinked with PEDOT:PSS, Si (OH)3
Hydrolysate terminal hydroxy group-OH the condensation cross-linking of group and tetraalkoxy compound forms firm O-Si-0 key, thus formed it is organic-
Inorganic hybridization system greatlys improve the hardening effect of antistatic coating.
Antistatic coating provided by the present invention is coated on substrate surface, obtains having both high-hardness, wearable by heat cure
With the antistatic coating of low square resistance；Meanwhile antistatic coating of the invention also has the characteristics that light transmittance is high.
[specific embodiment]
In order to make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with specific embodiment, to this
Invention is further elaborated.It should be appreciated that described herein, specific examples are only used to explain the present invention, and does not have to
It is of the invention in limiting.
Embodiment 1
A kind of antistatic coating, by mass percentage, including following component:
The PEDOT:PSS dispersion liquid is poly- (3,4- ethene dioxythiophene): the aqueous dispersion of poly- (styrene sulfonate).
Preparation method is as follows:
S1: the preparation of pre-hydrolyzed solution: PEDOT:PSS dispersion liquid is added to the container, sequentially adds deionization while stirring
Water, fluorocarbon surfactant, ethyl alcohol, ethylene glycol, 3- glycidyl ether oxygen propyl trimethoxy silicane, stir evenly, and are made pre-
Hydrolyzate；
S2: the preparation of antistatic coating: using pre-hydrolyzed solution obtained in S1 as presoma, being added in thermostat water bath,
60 DEG C are warming up to, tetraethyl orthosilicate is added, hydrochloric acid is added dropwise while stirring, after then sealing simultaneously insulated and stirred 12h, stops stirring
And be cooled to room temperature, obtain antistatic coating.
Antistatic coating made from the present embodiment is subjected to correlated performance test, specific test mode is as follows:
One, the preparation of antistatic coating
Antistatic coating obtained by the present embodiment is spread evenly across the alkali-free glass (rising sun using OPS-18 bar coating device
Nitre 0.5mm, light transmittance 92.4%) on surface, alkali-free glass is put into infrared drying oven, the baking-curing at 120 DEG C
20min forms antistatic coating on alkali-free glass surface, antistatic coating print is made.
Two, sheet resistance, light transmittance, the hardness, adhesive force, ethanol-tolerant wiping, resistance to white spirit of the antistatic coating print are measured
Improving soaking, and it is as follows to carry out performance test and ultraviolet ageing test, properties test method under the conditions of high temperature and humidity:
1, sheet resistance
Above-mentioned antistatic coating print is taken, is directly detected using impedance analyzer.
2, light transmittance
It is carried out by the regulation of method A in GB/T 2410-2008.
3, adhesive force
It is carried out by method as defined in ASTM D3359-09.
4, pencil hardness
It is carried out by method as defined in GB/T 6739.
5, scratch resistance
It carries out wiping reciprocal 1000 times on antistatic coating print with 1kg power using 0000# steel wool.
6, ethanol-tolerant wipes
It carries out wiping reciprocal 200 times on antistatic coating print using spirituous non-dust cloth is dipped in.
7, resistance to white spirit impregnates
Antistatic coating print steeps in white appliances oil solvent 2 hours, then takes out wiped clean.
8, high temperature and humidity is tested
By antistatic coating print temperature be adjusted to 85 DEG C, relative humidity be adjusted in 85% constant temperature humidity chamber,
It is taken out after 240h, then is cooled to room temperature and removes moisture content in 130 DEG C of dry 3min, then carry out testing impedance, impedance detecting method is such as
Impedance detecting method above-mentioned is identical.
9, salt spray test
5% sodium chloride concentration after attaching, 35 DEG C of temperature, salt mist tester store 48h under spray environment.
10, ultraviolet ageing is tested
Test condition setting:
1. UV lamp tube wave is long: 340nm
2. intensity of illumination: 2.0W/m2/ nm,
3. single cycle condition: 8 hours UV (60 DEG C of blackboard temperature), condensation (50 DEG C of blackboard temperature) in 4 hours；
Antistatic coating print is put into 192h in ultraviolet ageing test machine, is taken out, dry 3min removes water at 130 DEG C
Part, then carry out testing impedance；
Correlated performance test result such as table 1.
The preparation of antistatic coating print and the above properties are tested in used equipment in the present embodiment, infrared
Drying box is the infrared drying oven of the model HT-H-420 of Dongguan Hui Tai Machinery Co., Ltd. production；What impedance analyzer used
It is (setting HIOKI SM7110 day) high resistant instrument；Constant temperature humidity chamber is the model of the learned Industrial Co., Ltd.'s production in Dongguan
The constant temperature humidity chamber of BYTH-21C；Salt spray test machine is the KZ-120 salt spray test machine that Dongguan section is just producing；Ultraviolet ageing
Test machine is the ultraviolet ageing test machine of the model HT-UV-1300 of Dongguan City Hui Tai Machinery Co., Ltd. production.
Embodiment 2
A kind of antistatic coating, by mass percentage, including following components:
The PEDOT:PSS dispersion liquid is poly- (3,4- ethene dioxythiophene): the aqueous dispersion of poly- (styrene sulfonate).
The antistatic coating preparation method of the present embodiment is same as Example 1, wherein is warming up to 100 DEG C in S2 and keeps the temperature
It is cooling after being stirred to react 10h, antistatic coating is obtained, tests each of the present embodiment antistatic coating in the manner of example 1
Item performance, test result such as table 1.
Embodiment 3
A kind of antistatic coating, by mass percentage, including following components:
The PEDOT:PSS dispersion liquid is poly- (3,4- ethene dioxythiophene): the aqueous dispersion of poly- (styrene sulfonate).
The antistatic coating preparation method of the present embodiment is same as Example 1, wherein is warming up to 80 DEG C in S2 and keeps the temperature and stirs
It is cooling after mixing reaction 20h, antistatic coating is obtained, tests the items of the present embodiment antistatic coating in the manner of example 1
Performance, test result such as table 1.
Embodiment 4
A kind of antistatic coating, by mass percentage, including following component:
The PEDOT:PSS dispersion liquid is poly- (3,4- ethene dioxythiophene): the aqueous dispersion of poly- (styrene sulfonate).
The antistatic coating preparation method of the present embodiment is same as Example 1, tests the present embodiment in the manner of example 1
The properties of antistatic coating, test result such as table 1.
Embodiment 5
A kind of antistatic coating, by mass percentage, including following component:
The PEDOT:PSS dispersion liquid is poly- (3,4- ethene dioxythiophene): the aqueous dispersion of poly- (styrene sulfonate).
The antistatic coating preparation method of the present embodiment is same as Example 1, tests the present embodiment in the manner of example 1
The properties of antistatic coating, test result such as table 1.
Embodiment 6
A kind of antistatic coating, by mass percentage, including following component:
The PEDOT:PSS dispersion liquid is poly- (3,4- ethene dioxythiophene): the aqueous dispersion of poly- (styrene sulfonate).
The antistatic coating preparation method of the present embodiment is same as Example 1, tests the present embodiment in the manner of example 1
The properties of antistatic coating, test result such as table 1.
Embodiment 7
A kind of antistatic coating, by mass percentage, including following component:
The PEDOT:PSS dispersion liquid is poly- (3,4- ethene dioxythiophene): the aqueous dispersion of poly- (styrene sulfonate).
The antistatic coating preparation method of the present embodiment is same as Example 1, tests the present embodiment in the manner of example 1
The properties of antistatic coating, test result such as table 1.
Comparative example 1
A kind of antistatic coating, by mass percentage, including following components:
The PEDOT:PSS dispersion liquid is poly- (3,4- ethene dioxythiophene): the aqueous dispersion of poly- (styrene sulfonate).
Preparation method is identical as the preparation method of embodiment 1, and prepared antistatic coating properties are using implementation
The method of example 1 is tested, test result such as table 2.
Comparative example 2
The PEDOT:PSS dispersion liquid is poly- (3,4- ethene dioxythiophene): the aqueous dispersion of poly- (styrene sulfonate).
Preparation method is identical as the preparation method of embodiment 1, and prepared antistatic coating properties are using implementation
The method of example 1 is tested, test result such as table 2.
Comparative example 3
The PEDOT:PSS dispersion liquid is poly- (3,4- ethene dioxythiophene): the aqueous dispersion of poly- (styrene sulfonate).
Preparation method is identical as the preparation method of embodiment 1, and prepared antistatic coating properties are using implementation
The method of example 1 is tested, test result such as table 2.
Antistatic coating correlated performance test result prepared by 1 embodiment 1-7 of table
Antistatic coating correlated performance test result prepared by 2 comparative example 1-3 of table
According to the test result of table 1 it is found that the present invention is using PEDOT:PSS dispersion liquid as conductive component, with silane coupling agent
It is hydrolyzed to form presoma, be heated after tetraalkoxy compound is added, then is anti-made of hydrolysis under the catalysis of the catalyst
Electrostatic coatings, coated on can have very high hardness (reaching as high as 9H) and wearability, and sheet resistance after substrate surface and solidification
Low (minimum reachable 1.1 × 10^4 Ω/) also while guaranteeing other performances (performances such as light transmittance, adhesive force, ethanol-tolerant wiping)
It is excellent.
In addition, according to comparative example test result in table 2 it is found that the present invention is using PEDOT:PSS dispersion liquid as conductive component, with
Silane coupling agent is hydrolyzed to form presoma, heats after tetraalkoxy compound is added, then water under the catalysis of the catalyst
Antistatic coating made of solving just has the excellent properties, and silane coupling agent, tetraalkoxy compound or catalyst lack one
Cause antistatic coating that effect of the invention is not achieved.
The above content is combine specific optimal technical scheme further detailed description of the invention, and it cannot be said that
Specific implementation of the invention is only limited to these instructions.For the professional technician of the technical field of the invention, In
Under the premise of not departing from present inventive concept, a number of simple deductions or replacements can also be made, all shall be regarded as belonging to of the invention
Protection scope.
Claims (8)
1. a kind of antistatic coating, which is characterized in that by mass percentage, including following components:
The PEDOT:PSS dispersion liquid is poly- (3,4- ethene dioxythiophene): the aqueous dispersion of poly- (styrene sulfonate).
2. antistatic coating according to claim 1, which is characterized in that the tetraalkoxy compound is positive silicic acid tetramethyl
One of or two or more mixture in ester, tetraethyl orthosilicate, positive silicic acid orthocarbonate and tetrabutyl silicate.
3. antistatic coating according to claim 1, which is characterized in that the silane coupling agent is 3- glycidyl ether oxygen
Propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, γ-mercaptopropyl trimethoxysilane, γ-
TSL 8330, γ aminopropyltriethoxy silane, vinyltrimethoxysilane, three ethoxy of vinyl
One of or two or more mixture in base silane.
4. antistatic coating according to claim 1, which is characterized in that the alcohols solvent is methanol, ethyl alcohol, trifluoro second
Alcohol, isopropanol, isobutanol, n-amyl alcohol, sec-amyl alcohol, one of or two or more mixture in diacetone alcohol.
5. antistatic coating according to claim 1, which is characterized in that the high boiling solvent is dimethyl sulfoxide, second
Glycol, propylene glycol, diethylene glycol (DEG), glycerine, formamide, one of or two or more mixing in n,N-Dimethylformamide
Object.
6. antistatic coating according to claim 1, which is characterized in that the surfactant is alkylphenol-polyethenoxy
Ethers ionic surface active agent, acetylenic diols surfactant and the one of which in fluorine carbon nonionic surfactant or two kinds
Above mixture.
7. antistatic coating according to claim 1, which is characterized in that the catalyst is formic acid, acetic acid, hydrochloric acid, nitre
Acid, sulfuric acid, one of or two or more mixture in oxalic acid.
8. such as the preparation method of the described in any item antistatic coatings of claim 1-7, which comprises the following steps:
S1: PEDOT:PSS dispersion liquid is added to the container, and sequentially adds deionized water, high boiling solvent, surface work while stirring
Property agent, alcohols solvent, silane coupling agent, stir evenly, be made pre-hydrolyzed solution；
S2: the pre-hydrolyzed solution is added in isothermal reaction container, and tetraalkoxy compound is added, is warming up to 60-100 DEG C, side
The side dropwise addition catalyst is stirred, after then sealing simultaneously insulated and stirred 10-20h, stopping is stirred and cooling, obtains antistatic painting
Material.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113512354A (en) * | 2021-09-13 | 2021-10-19 | 潍坊赛宝工业技术研究院有限公司 | Glass surface treatment material and preparation method thereof |
| CN115521702A (en) * | 2022-09-23 | 2022-12-27 | 湖南纳昇电子科技有限公司 | Anti-reflection high-hardness PEDOT (Poly ethylene glycol Ether-styrene) PSS (Poly ethylene-styrene) electronic coating as well as preparation method and application thereof |
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| CN107394135A (en) * | 2017-06-26 | 2017-11-24 | 中航锂电（洛阳）有限公司 | A kind of graphene-based composite negative pole material and preparation method thereof |
| CN109741853A (en) * | 2019-02-21 | 2019-05-10 | 珠海纳金科技有限公司 | A kind of silver nanowires coating fluid and preparation method thereof |
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| CN115521702A (en) * | 2022-09-23 | 2022-12-27 | 湖南纳昇电子科技有限公司 | Anti-reflection high-hardness PEDOT (Poly ethylene glycol Ether-styrene) PSS (Poly ethylene-styrene) electronic coating as well as preparation method and application thereof |
| CN115521702B (en) * | 2022-09-23 | 2023-10-17 | 湖南纳昇电子科技有限公司 | PEDOT (polyether urethane) PSS (polyphenylene sulfide) electronic coating capable of enhancing reflection and high in hardness as well as preparation method and application thereof |
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Application publication date: 20191122 |