CN107043585A - A kind of preparation method of conductive attapulgite antistatic coating - Google Patents

A kind of preparation method of conductive attapulgite antistatic coating Download PDF

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CN107043585A
CN107043585A CN201710274454.1A CN201710274454A CN107043585A CN 107043585 A CN107043585 A CN 107043585A CN 201710274454 A CN201710274454 A CN 201710274454A CN 107043585 A CN107043585 A CN 107043585A
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attapulgite
graphene
preparation
conductive
rotating speed
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张志军
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ANHUI BOSHUO TECHNOLOGY Co Ltd
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ANHUI BOSHUO TECHNOLOGY Co Ltd
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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
    • C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/0605—Polycondensates containing five-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms
    • C08G73/0611—Polycondensates containing five-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms with only one nitrogen atom in the ring, e.g. polypyrroles
    • 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
    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/65—Additives macromolecular
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

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Abstract

The invention discloses a kind of preparation method of conductive attapulgite antistatic coating, it includes the preparation of graphene coated attapulgite, the preparation of nano antimony tin oxide aqueous precursor gel, the preparation of attapulgite/graphene/nanometer tin-antiomony oxide composite, the step such as preparation, the preparation of antistatic coating of attapulgite/graphene/nanometer tin-antiomony oxide/polypyrrole conducing composite material material.The present invention forms graphene, nano antimony tin oxide, three layers of conductive layer of polypyrrole by attapulgite's surface and conductive attapulgite is made, then bisphenol A type epoxy resin is used for film forming matter, using conductive attapulgite as antistatic additive, adding the coating made from raw material such as hyper-dispersant, diluent, curing agent simultaneously not only has excellent antistatic behaviour, physical and mechanical properties, chemical proofing and weatherability, also with good ornamental and adhesive force.

Description

A kind of preparation method of conductive attapulgite antistatic coating
Technical field
The present invention relates to a kind of preparation method of antistatic coating, and in particular to a kind of conductive attapulgite antistatic coating Preparation method.
Background technology
Electrostatic is ubiquitous, either in industrial production and daily life, and electrostatic brings very big harm such as sometimes Tank truck, oil storage tank of transporting oil products etc., in order to eliminate electrostatic, people take various methods, wherein using antistatic coating Solve the problems, such as it is one of important means.Except electrostatic hazard is big in daily production and living, in terms of extraordinary workpiece, such as fly at a high speed High-speed flight produces substantial amounts of electrostatic to row device with windage in atmosphere, if eliminated not in time, produces discharge band and comes very big Harm.Therefore, antistatic coating arises at the historic moment.Antistatic coating is with conductive and exclusion accumulation electrostatic charge ability function Property coating, its surface resistivity is 106-109Between Ω, electric current can be quickly conducted, electrostatic charge is eliminated.It is in the market to use more Carbon-based material (carbon black, graphite etc.), metal dust (silver powder, copper powder, nickel powder etc.), metal oxide semiconductor (tin oxide, oxidation Iron, zinc oxide), conducting nanoparticles and antistatic auxiliary agent be added to as conductive filler in coating and realize anlistatig performance, Or antistatic coating is used as using conducting high polymers things such as polyacetylene, polyaniline, polypyrrole, polyparaphenylene, polythiophenes Film forming matter, yet there are no mutually compound obtained conductive recessed with graphene, nano antimony tin oxide, polypyrrole using attapulgite Convex rod soil is applied to antistatic coating as antistatic additive.Therefore, the present invention develops a kind of antistatic painting of conductive attapulgite The preparation method of material.
The content of the invention
It is an object of the invention to provide a kind of preparation method of conductive attapulgite antistatic coating, the present invention is by recessed The native surface of convex rod forms graphene, nano antimony tin oxide, three layers of conductive layer of polypyrrole and conductive attapulgite is made, and then uses Bisphenol A type epoxy resin is film forming matter, using conductive attapulgite as antistatic additive, while adding hyper-dispersant, diluent, solidification Coating made from the raw materials such as agent not only has excellent antistatic behaviour, physical and mechanical properties, chemical proofing and weatherability, also With good ornamental and adhesive force.
To achieve the above object, the present invention is adopted the following technical scheme that：
A kind of preparation method of conductive attapulgite antistatic coating, comprises the following steps：
（1）According to mass ratio 1:5-10 weighs graphene oxide and attapulgite, then according to solid-to-liquid ratio 1:30-40 will aoxidize stone Black alkene adds volume fraction in 20-30% ethanol water, ultrasonic disperse 20-40min obtains graphene oxide dispersion, then 300- is placed in after attapulgite, ultrasonic disperse 30-50min, high-purity argon gas purging 1-2h are added into graphene oxide dispersion Under 500W iodine-tungsten lamps and configure 420nm cut-off type optical filter filter off ultraviolet light, open light source carry out photo catalytic reduction graphene Light source is closed after cladding, irradiation 2-3h, suction filtration, filter cake is washed 3-4 times with deionized water and absolute ethyl alcohol successively, at 60-70 DEG C 5-7h is dried, is ground, sieving produces graphene coated attapulgite；
（2）According to mass ratio 1:0.05-0.15 is by SnCl4·5H2O and SbCl3It is well mixed, then according to solid-to-liquid ratio 1:20-30 Add mixture in absolute ethyl alcohol, the Macrogol 600 equivalent to mixture quality 3-5% is added after stirring, and Solution PH=2-3 is adjusted for 25% ammonia spirit with mass fraction, 30- is stirred with 1500-2500r/min rotating speed at room temperature 50min, still aging 5-10h, centrifuge jello, remove after supernatant liquor, are washed, then centrifuged again with ethanol, Repeated washing is centrifuged 3-4 times, obtains nano antimony tin oxide aqueous precursor gel；
（3）According to mass ratio 1:0.4-0.6 mixes nano antimony tin oxide aqueous precursor gel and graphene coated attapulgite, 15-30min is stirred under 3000-5000r/min rotating speed, supercritical CO is then carried out2Dry, dry after the completion of with 5-7 DEG C/ Min speed is warming up to 590-630 DEG C, is incubated 1-3h, is cooled to room temperature, obtains attapulgite/graphene/nanometer tin-antiomony oxide Composite；
（4）Quality is made according to attapulgite obtained above/graphene/nanometer tin-antiomony oxide composite ultrasonic agitation that adds water Fraction is 15-20% slurries；Then add equivalent to attapulgite/graphene/nanometer tin-antiomony oxide composite quality 40-50% pyrroles and 30-40% dodecyl sodium sulfate, 5-10min is stirred under 1500-2000r/min rotating speed；Finally In the water for dissolving ammonium persulfate into 30-40 times of quality, the mol ratio of ammonium persulfate and pyrroles are 1.5-2.5:1, then be rapidly added Into above-mentioned slurries under 20-30 DEG C of temperature and 2000-3000r/min rotating speed stirring reaction 1-2h, suction filtration, and spend from Sub- water washing to filtrate is colourless, by filter cake in drying 2-4h at 80-90 DEG C, is ground, and sieving produces required conductive concave convex rod Soil；
（5）The conductive attapulgite of 30-45 parts by weight of bisphenol A types epoxy resin 621,10-15 parts by weight, 2-4 parts by weight is weighed to surpass Dispersant 32500,15-25 parts by weight of xylene, 5-10 part by weight of n-butanol, above-mentioned raw materials are well mixed, then in 3000- Fineness≤30 μm are ground under 5000r/min rotating speed, the cashew nut oil modified phenolic aldehyde amine of 15-25 parts by weight are added, in 500- 10-30min is stirred under 1500r/min rotating speed, standing goes after bubble removing to produce coating finished product.
Step（1）Described in graphene oxide using improve Hummers methods be prepared.
Step（1）Described in ultrasonic power be 200-300W.
Step（2）Described in centrifugation rotating speed be 4000-6000r/min, the time is 20-40min.
Step（3）Described in supercritical CO2Drying condition is：Supercritical CO2Flow be 20-30ml/min, temperature is 50-65 DEG C, pressure is 15-20MPa, and drying time is 3-5h.
Step（4）Described in ultrasonic power be 250-350W.
Beneficial effects of the present invention：
The present invention is coated using photo catalytic reduction graphene oxide to attapulgite so that in attapulgite's surface formation stone The black conductive layer of alkene first, then using sol-gel process in graphene coated attapulgite's surface formation nano antimony tin oxide the Two conductive layers, finally form poly- pyrrole using situ aggregation method in attapulgite/graphene/nanometer tin-antiomony oxide composite material surface The 3rd conductive layer is coughed up, conductive attapulgite is obtained, bisphenol A type epoxy resin is then used for film forming matter, with conductive attapulgite For antistatic additive, at the same add the coating made from raw material such as hyper-dispersant, diluent, curing agent not only have it is excellent antistatic Property, physical and mechanical properties, chemical proofing and weatherability, also with good ornamental and adhesive force.
Embodiment
Embodiment 1
A kind of preparation method of conductive attapulgite antistatic coating, comprises the following steps：
（1）According to mass ratio 1:5 weigh graphene oxide and attapulgite, then according to solid-to-liquid ratio 1:30 add graphene oxide Enter in the ethanol water that volume fraction is 20%, ultrasonic disperse 20min obtains graphene oxide dispersion, then to graphene oxide Added in dispersion liquid after attapulgite, ultrasonic disperse 30min, high-purity argon gas purging 1h and be placed under 300W iodine-tungsten lamps and configure 420nm cut-off type optical filter filters off ultraviolet light, opens after light source carries out photo catalytic reduction graphene coated, irradiation 3h and closes light Source, suction filtration, filter cake is washed 3 times with deionized water and absolute ethyl alcohol successively, in 60 DEG C of dry 7h, is ground, and sieving produces graphene Coat attapulgite；
（2）According to mass ratio 1:0.05 by SnCl4·5H2O and SbCl3It is well mixed, then according to solid-to-liquid ratio 1:20 by mixture It is added in absolute ethyl alcohol, the Macrogol 600 equivalent to mixture quality 3-5% is added after stirring, and divided with quality Number is 25% ammonia spirit regulation solution PH=2, stirs 50min, still aging 5h at room temperature with 1500r/min rotating speed, Jello is centrifuged, is removed after supernatant liquor, is washed, then centrifuged again with ethanol, repeated washing is centrifuged 3 times, is obtained Nano antimony tin oxide aqueous precursor gel；
（3）According to mass ratio 1:0.4 mixes nano antimony tin oxide aqueous precursor gel and graphene coated attapulgite, 30min is stirred under 3000r/min rotating speed, supercritical CO is then carried out2Dry, with 5 DEG C/min speed liter after the completion of drying Temperature is incubated 3h, is cooled to room temperature, obtains attapulgite/graphene/nanometer tin-antiomony oxide composite to 590 DEG C；
（4）Quality is made according to attapulgite obtained above/graphene/nanometer tin-antiomony oxide composite ultrasonic agitation that adds water Fraction is 15% slurries；Then add equivalent to attapulgite/graphene/nanometer tin-antiomony oxide composite quality 40% Pyrroles and 30% dodecyl sodium sulfate, 10min is stirred under 1500r/min rotating speed；Finally dissolve ammonium persulfate into 30 times In the water of quality, the mol ratio of ammonium persulfate and pyrroles are 1.5:1, then be quickly adding into above-mentioned slurries in 20 DEG C of temperature and Stirring reaction 2h, suction filtration under 2000r/min rotating speed, and it is colourless to be washed with deionized to filtrate, by filter cake at 80 DEG C 4h is dried, is ground, sieving produces required conductive attapulgite；
（5）Weigh the conductive attapulgite of 30 parts by weight of bisphenol A types epoxy resin 621,10 parts by weight, 2 parts by weight hyper-dispersants 32500th, 15 parts by weight of xylene, 5 part by weight of n-butanol, above-mentioned raw materials are well mixed, then under 3000r/min rotating speed Fineness≤30 μm are ground to, the cashew nut oil modified phenolic aldehyde amine of 15 parts by weight is added, stirred under 500r/min rotating speed 30min, standing goes after bubble removing to produce coating finished product.
Step（1）Described in graphene oxide using improve Hummers methods be prepared.
Step（1）Described in ultrasonic power be 300W.
Step（2）Described in centrifugation rotating speed be 4000r/min, the time is 40min.
Step（3）Described in supercritical CO2Drying condition is：Supercritical CO2Flow be 20ml/min, temperature is 50 DEG C, pressure is 15MPa, and drying time is 5h.
Step（4）Described in ultrasonic power be 250W.
Embodiment 2
A kind of preparation method of conductive attapulgite antistatic coating, comprises the following steps：
（1）According to mass ratio 1:8 weigh graphene oxide and attapulgite, then according to solid-to-liquid ratio 1:35 add graphene oxide Enter in the ethanol water that volume fraction is 25%, ultrasonic disperse 30min obtains graphene oxide dispersion, then to graphene oxide Added in dispersion liquid after attapulgite, ultrasonic disperse 40min, high-purity argon gas purging 1.5h and be placed under 400W iodine-tungsten lamps and configure 420nm cut-off type optical filter filters off ultraviolet light, opens after light source carries out photo catalytic reduction graphene coated, irradiation 2.5h and closes Light source, suction filtration, filter cake is washed 3 times with deionized water and absolute ethyl alcohol successively, in 65 DEG C of dry 6h, is ground, and sieving produces graphite Alkene coats attapulgite；
（2）According to mass ratio 1:0.1 by SnCl4·5H2O and SbCl3It is well mixed, then according to solid-to-liquid ratio 1:25 by mixture It is added in absolute ethyl alcohol, the Macrogol 600 equivalent to mixture quality 4% is added after stirring, and use mass fraction Solution PH=2.5 are adjusted for 25% ammonia spirit, 40min, still aging 8h are stirred with 2000r/min rotating speed at room temperature, Jello is centrifuged, is removed after supernatant liquor, is washed, then centrifuged again with ethanol, repeated washing is centrifuged 3 times, is obtained Nano antimony tin oxide aqueous precursor gel；
（3）According to mass ratio 1:0.5 mixes nano antimony tin oxide aqueous precursor gel and graphene coated attapulgite, 25min is stirred under 4000r/min rotating speed, supercritical CO is then carried out2Dry, with 6 DEG C/min speed liter after the completion of drying Temperature is incubated 2h, is cooled to room temperature, obtains attapulgite/graphene/nanometer tin-antiomony oxide composite to 610 DEG C；
（4）Quality is made according to attapulgite obtained above/graphene/nanometer tin-antiomony oxide composite ultrasonic agitation that adds water Fraction is 18% slurries；Then add equivalent to attapulgite/graphene/nanometer tin-antiomony oxide composite quality 45% Pyrroles and 35% dodecyl sodium sulfate, 8min is stirred under 1800r/min rotating speed；Finally dissolve ammonium persulfate into 35 times In the water of quality, the mol ratio of ammonium persulfate and pyrroles are 2:1, then be quickly adding into above-mentioned slurries in 25 DEG C of temperature and Stirring reaction 1.5h, suction filtration under 2500r/min rotating speed, and it is colourless to be washed with deionized to filtrate, by filter cake in 85 DEG C Lower dry 3h, grinds, and sieving produces required conductive attapulgite；
（5）Weigh the conductive attapulgite of 42 parts by weight of bisphenol A types epoxy resin 621,12 parts by weight, 3 parts by weight hyper-dispersants 32500th, 20 parts by weight of xylene, 8 part by weight of n-butanol, above-mentioned raw materials are well mixed, then under 4000r/min rotating speed Fineness≤30 μm are ground to, the cashew nut oil modified phenolic aldehyde amine of 20 parts by weight is added, stirred under 1000r/min rotating speed 20min, standing goes after bubble removing to produce coating finished product.
Step（1）Described in graphene oxide using improve Hummers methods be prepared.
Step（1）Described in ultrasonic power be 250W.
Step（2）Described in centrifugation rotating speed be 5000r/min, the time is 30min.
Step（3）Described in supercritical CO2Drying condition is：Supercritical CO2Flow be 25ml/min, temperature is 55 DEG C, pressure is 18MPa, and drying time is 4h.
Step（4）Described in ultrasonic power be 300W.
Embodiment 3
A kind of preparation method of conductive attapulgite antistatic coating, comprises the following steps：
（1）According to mass ratio 1:10 weigh graphene oxide and attapulgite, then according to solid-to-liquid ratio 1:40 by graphene oxide Volume fraction is added in 30% ethanol water, ultrasonic disperse 40min obtains graphene oxide dispersion, then to graphite oxide Added in alkene dispersion liquid after attapulgite, ultrasonic disperse 50min, high-purity argon gas purging 2h and be placed under 500W iodine-tungsten lamps and configure 420nm cut-off type optical filter filters off ultraviolet light, opens after light source carries out photo catalytic reduction graphene coated, irradiation 2h and closes light Source, suction filtration, filter cake is washed 4 times with deionized water and absolute ethyl alcohol successively, in 70 DEG C of dry 5h, is ground, and sieving produces graphene Coat attapulgite；
（2）According to mass ratio 1:0.15 by SnCl4·5H2O and SbCl3It is well mixed, then according to solid-to-liquid ratio 1:30 by mixture It is added in absolute ethyl alcohol, the Macrogol 600 equivalent to mixture quality 5% is added after stirring, and use mass fraction Solution PH=3 are adjusted for 25% ammonia spirit, 30min, still aging 10h are stirred with 2500r/min rotating speed at room temperature, from Heart separating gel thing, is removed after supernatant liquor, is washed, then centrifuged again with ethanol, and repeated washing is centrifuged 4 times, is received Rice tin-antiomony oxide aqueous precursor gel；
（3）According to mass ratio 1:0.6 mixes nano antimony tin oxide aqueous precursor gel and graphene coated attapulgite, 15min is stirred under 5000r/min rotating speed, supercritical CO is then carried out2Dry, with 7 DEG C/min speed liter after the completion of drying Temperature is incubated 1h, is cooled to room temperature, obtains attapulgite/graphene/nanometer tin-antiomony oxide composite to 630 DEG C；
（4）Quality is made according to attapulgite obtained above/graphene/nanometer tin-antiomony oxide composite ultrasonic agitation that adds water Fraction is 20% slurries；Then add equivalent to attapulgite/graphene/nanometer tin-antiomony oxide composite quality 50% Pyrroles and 40% dodecyl sodium sulfate, 5min is stirred under 2000r/min rotating speed；Finally dissolve ammonium persulfate into 40 times In the water of quality, the mol ratio of ammonium persulfate and pyrroles are 2.5:1, then be quickly adding into above-mentioned slurries in 30 DEG C of temperature and Stirring reaction 1h, suction filtration under 3000r/min rotating speed, and it is colourless to be washed with deionized to filtrate, by filter cake at 90 DEG C 2h is dried, is ground, sieving produces required conductive attapulgite；
（5）Weigh the conductive attapulgite of 45 parts by weight of bisphenol A types epoxy resin 621,15 parts by weight, 4 parts by weight hyper-dispersants 32500th, 25 parts by weight of xylene, 10 part by weight of n-butanol, above-mentioned raw materials are well mixed, then in 5000r/min rotating speed Under be ground to fineness≤30 μm, add the cashew nut oil modified phenolic aldehyde amine of 25 parts by weight, under 1500r/min rotating speed stir 10min, standing goes after bubble removing to produce coating finished product.
Step（1）Described in graphene oxide using improve Hummers methods be prepared.
Step（1）Described in ultrasonic power be 200W.
Step（2）Described in centrifugation rotating speed be 6000r/min, the time is 20min.
Step（3）Described in supercritical CO2Drying condition is：Supercritical CO2Flow be 30ml/min, temperature is 65 DEG C, pressure is 20MPa, and drying time is 3h.
Step（4）Described in ultrasonic power be 350W.

Claims (6)

1. a kind of preparation method of conductive attapulgite antistatic coating, it is characterised in that comprise the following steps：
(1) according to mass ratio 1:5-10 weighs graphene oxide and attapulgite, then according to solid-to-liquid ratio 1:30-40 will aoxidize stone Black alkene adds volume fraction in 20-30% ethanol water, ultrasonic disperse 20-40min obtains graphene oxide dispersion, then 300- is placed in after attapulgite, ultrasonic disperse 30-50min, high-purity argon gas purging 1-2h are added into graphene oxide dispersion Under 500W iodine-tungsten lamps and configure 420nm cut-off type optical filter filter off ultraviolet light, open light source carry out photo catalytic reduction graphene Light source is closed after cladding, irradiation 2-3h, suction filtration, filter cake is washed 3-4 times with deionized water and absolute ethyl alcohol successively, at 60-70 DEG C 5-7h is dried, is ground, sieving produces graphene coated attapulgite；
(2) according to mass ratio 1:0.05-0.15 is by SnCl4·5H2O and SbCl3It is well mixed, then according to solid-to-liquid ratio 1:20-30 Add mixture in absolute ethyl alcohol, the Macrogol 600 equivalent to mixture quality 3-5% is added after stirring, and Solution PH=2-3 is adjusted for 25% ammonia spirit with mass fraction, 30- is stirred with 1500-2500r/min rotating speed at room temperature 50min, still aging 5-10h, centrifuge jello, remove after supernatant liquor, are washed, then centrifuged again with ethanol, Repeated washing is centrifuged 3-4 times, obtains nano antimony tin oxide aqueous precursor gel；
(3) according to mass ratio 1:0.4-0.6 mixes nano antimony tin oxide aqueous precursor gel and graphene coated attapulgite, 15-30min is stirred under 3000-5000r/min rotating speed, supercritical CO is then carried out2Dry, dry after the completion of with 5-7 DEG C/ Min speed is warming up to 590-630 DEG C, is incubated 1-3h, is cooled to room temperature, obtains attapulgite/graphene/nanometer tin-antiomony oxide Composite；
(4) quality is made according to attapulgite obtained above/graphene/nanometer tin-antiomony oxide composite ultrasonic agitation that adds water Fraction is 15-20% slurries；Then add equivalent to attapulgite/graphene/nanometer tin-antiomony oxide composite quality 40-50% pyrroles and 30-40% dodecyl sodium sulfate, 5-10min is stirred under 1500-2000r/min rotating speed；Finally In the water for dissolving ammonium persulfate into 30-40 times of quality, the mol ratio of ammonium persulfate and pyrroles are 1.5-2.5:1, then be rapidly added Into above-mentioned slurries under 20-30 DEG C of temperature and 2000-3000r/min rotating speed stirring reaction 1-2h, suction filtration, and spend from Sub- water washing to filtrate is colourless, by filter cake in drying 2-4h at 80-90 DEG C, is ground, and sieving produces required conductive concave convex rod Soil；
(5) the conductive attapulgite of 30-45 parts by weight of bisphenol A types epoxy resin 621,10-15 parts by weight, 2-4 parts by weight is weighed to surpass Dispersant 32500,15-25 parts by weight of xylene, 5-10 part by weight of n-butanol, above-mentioned raw materials are well mixed, then in 3000- Fineness≤30 μm are ground under 5000r/min rotating speed, the cashew nut oil modified phenolic aldehyde amine of 15-25 parts by weight are added, in 500- 10-30min is stirred under 1500r/min rotating speed, standing goes after bubble removing to produce coating finished product.
2. a kind of preparation method of conductive attapulgite antistatic coating according to claim 1, it is characterised in that step （1）Described in graphene oxide using improve Hummers methods be prepared.
3. a kind of preparation method of conductive attapulgite antistatic coating according to claim 1, it is characterised in that step （1）Described in ultrasonic power be 200-300W.
4. a kind of preparation method of conductive attapulgite antistatic coating according to claim 1, it is characterised in that step （2）Described in centrifugation rotating speed be 4000-6000r/min, the time is 20-40min.
5. a kind of preparation method of conductive attapulgite antistatic coating according to claim 1, it is characterised in that step （3）Described in supercritical CO2Drying condition is：Supercritical CO2Flow be 20-30ml/min, temperature be 50-65 DEG C, pressure For 15-20MPa, drying time is 3-5h.
6. a kind of preparation method of conductive attapulgite antistatic coating according to claim 1, it is characterised in that step （4）Described in ultrasonic power be 250-350W.
CN201710274454.1A 2017-04-25 2017-04-25 A kind of preparation method of conductive attapulgite antistatic coating Pending CN107043585A (en)

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Cited By (3)

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CN107629511A (en) * 2017-10-27 2018-01-26 桂林市漓江机电制造有限公司 A kind of multi-functional UV coating
CN108863312A (en) * 2018-07-12 2018-11-23 李磊 A kind of Antistatic ceramic high performance antistatic agent and preparation method thereof
CN111703167A (en) * 2020-06-28 2020-09-25 广东裕泰实业有限公司 High-antistatic modified polymer insulating material and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107629511A (en) * 2017-10-27 2018-01-26 桂林市漓江机电制造有限公司 A kind of multi-functional UV coating
CN108863312A (en) * 2018-07-12 2018-11-23 李磊 A kind of Antistatic ceramic high performance antistatic agent and preparation method thereof
CN111703167A (en) * 2020-06-28 2020-09-25 广东裕泰实业有限公司 High-antistatic modified polymer insulating material and preparation method thereof

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