CN104710908A - Special anticorrosion conductive powder coating for vertical shaft fluidized bed dip-coating as well as preparation method and application of coating - Google Patents
Special anticorrosion conductive powder coating for vertical shaft fluidized bed dip-coating as well as preparation method and application of coating Download PDFInfo
- Publication number
- CN104710908A CN104710908A CN201510128721.5A CN201510128721A CN104710908A CN 104710908 A CN104710908 A CN 104710908A CN 201510128721 A CN201510128721 A CN 201510128721A CN 104710908 A CN104710908 A CN 104710908A
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- Prior art keywords
- coating
- vertical shaft
- fluidized bed
- powder
- conductive
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- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
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- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
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- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- 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
- 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
- C09D163/04—Epoxynovolacs
-
- 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
- C09D163/10—Epoxy resins modified by unsaturated compounds
-
- 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
- C09D5/03—Powdery paints
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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
- C09D5/08—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
- C09D5/24—Electrically-conducting paints
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Paints Or Removers (AREA)
Abstract
The invention relates to a special anticorrosion conductive powder coating for vertical shaft fluidized bed dip-coating. The special anticorrosion conductive powder coating is prepared from the following raw materials in parts by weight: 500-900 parts of film-forming resin and curing agent, 0-200 parts of glass flakes, 0-350 parts of filler, 15-50 parts of auxiliaries, 5-100 parts of conductive material and 1-5 parts of nanometer aluminum oxide or nano fumed silica. The powder coating has the characteristics of a high glass transition temperature, low specific gravity which is generally less than or equal to 1.1g/cm<3>, and easiness for fluidization; even though hundreds of tons of powder is added to a 20m deep well, the powder can be fluidized easily and uniformly; in case of too high specific gravity and difficult fluidization, the vertical shaft dip-coating method can not be utilized; the powder aims at a hot-dip coating construction process, and the film formed by the coating has surface conduction characteristics and high temperature water boiling resistance, and therefore, the coating is suitable for anti-corrosion coating of long linear workpieces such as mine mining anti-explosion gas pipelines, natural gas pipelines and liquefied gas pipelines; the coating is adaptive to the vertical shaft fluidized beds as deep as 20m, and still has good fluidity, which cannot be realized by common powders easily.
Description
Technical field
The invention belongs to powder coating technology field, particularly a kind of Functional Powder Coating, especially a kind of vertical shaft fluidized bed dipping special anti-corrosion conductive powder paint and preparation method and application.
Background technology
China such as to send need to use anticorrosion conductive conduits in a large number at the field in mine excavation, natural gas transport, Chemical Manufacture, western gas east, these pipelines all need to lead and destatic and flame retardant resistance.Because pipe diameter is general comparatively large and single pipe is often very long, much suitable coating process is also developed, and is 3PE pipeline, 2PE pipeline the earliest, and developing into now clinkery epoxy powder coating pipeline is main flow.Vertical shaft dip-coating conduction flame retardant type clinkery epoxy powder coating is at present by the solution affirmed.The application of vertical shaft fluidized-bed dipping has significant advantage: except coating performance excellence, utilization ratio, saving power and preventing pollution dye, the low cost of high, the coating 100% of coating efficiency, be easy to the features such as automation paint, very soon by pipe production transport enterprise is accepted.
Vertical shaft fluidized bed dipping technique, due to well depth comparatively dark (general 6-20 meters dark), fluid effect problem is difficult to solve, require that powder will be easy to fluidisation, also will realize the features such as high temperature resistant not conglomeration, not sagging, any surface finish, conductive effect be remarkable, these all need ultimate attainment from the selection of coating, controlling of production process, quality examination checking on, ready-made electro-conductive material and impregnating material selection, lower powder coating density (light specific gravity), higher second-order transition temperature (TG value), suitable size-grade distribution, perfect detection means etc.Current existing powder coating all can not meet above-mentioned requirements, and fluid effect is bad, can not meet existing user demand.
By retrieval, not yet find the patent publication us relevant to patent application of the present invention.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art part, there is provided a kind of there is high glass transition temperature, light specific gravity, be easy to the feature of fluidisation, also can fluidisation be even easily even if add up to a hundred tons of powder in 20 meters of deep-wells, coating has preparation method and the application of the vertical shaft fluidized bed dipping special anti-corrosion conductive powder paint of surface conduction characteristic and high temperature resistant poach characteristic after becoming paint film, this preparation method is simple, easy to operate, save production cost, improve the economic benefit of enterprise.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of vertical shaft fluidized bed dipping special anti-corrosion conductive powder paint, its raw material forms component and parts by weight are:
And its raw material forms component and parts by weight are:
And described film-forming resin and solidifying agent are the one in the collocation of following category:
(1) epoxy resin+phenols curing agent+imidazole and its derivants system, mass ratio is (50-70): (12-16): (3-8);
(2) epoxy resin+polyester resin system, mass ratio is 50:50 or 60:40 or 70:30 or 80:20;
(3) urethane+different fluorine that ketone isocyanate systems, mass ratio is 80:20;
(4) Epocryl+long chain dicarboxylic acid system, mass ratio is 80-83:17-20;
(5) epoxy resin+polyamine+imidazole and its derivants system;
(6) thermoplastic resin system.
And the fineness of described glass flake is 200-1000 order; Or described filler is one or more mixtures in process white, ultra-fine barium sulfate, activared carbon sulfur barium, basalt chopped fiber powder, silicon-dioxide, wollastonite powder, silicon powder, mica powder, sericite.
And described auxiliary agent is mixture, its composition and parts by weight are:
Butyl polyacrylate flow agent: 16 ~ 22 parts;
Brightening agent: 10 ~ 20 parts;
Defoamer or st-yrax: 4 ~ 8 parts;
Be mixed into a kind of raw material in this ratio, and then press formula rate weighing use.
And described electro-conductive material is for can realize coatingsurface resistance 1 × 10
3---1 × 10
9the electro-conductive material of ohm.
And described electro-conductive material is one or more mixture in conductive carbon black, conductive carbon nanotube, electrically conductive graphite, conductive mica powder, conductive metal powder, electrically conductive polyaniline.
The preparation method of vertical shaft fluidized bed dipping special anti-corrosion conductive powder paint as above, step is as follows:
By film-forming resin and solidifying agent, glass flake, filler, auxiliary agent and electro-conductive material precise, drop in agitator, mix 6-15 minutes, after fully mixing, be discharged in the hopper of double-screw type forcing machine, forcing machine one district temperature 90-95 is spent, two district's temperature 100-105 are spent, and screw speed 350-450 revs/min, extrudes, cooling compressing tablet, obtains normal temperature tablet;
Then normal temperature tablet and nano aluminium oxide or nano fumed silica are mixed even, enter again in pulverizer and carry out micronizing, sieve, control particle size range at D50=35-50, then test following index: dry powder flow, surface resistivity, tracking index, pliability test, cathodic disbonding test, flame retardant properties test, pipe flatten coating test etc.; All qualifiedly namely obtain vertical shaft fluidized bed dipping special anti-corrosion conductive powder paint.
And step is as follows:
(1) described electro-conductive material is polyaniline, and its preparation process is as follows:
1. emulsion polymerization synthesized polyaniline technique: add in the reactor in aniline: the ratio of the amount of substance of dodecylbenzene is that the ratio of 2:1 is for adding aniline and dodecylbenzene, water, dimethylbenzene is added successively after mixing, abundant stirring, to obtaining transparent emulsion;
2. then in transparent emulsion in ammonium persulphate: the ratio of the amount of substance of aniline is that the ratio of 1:1 drips ammonium persulphate (NH
4)
2s
2o
8the aqueous solution, system color slowly deepens, and keeps system temperature 0 ~ 20 DEG C, continues stirring 30 minutes, after during static storing 24, then adds acetone breakdown of emulsion, with ethanol or acetone repetitive scrubbing 3 ~ 4 times, removes ethanol or acetone, filters and to obtain precipitation;
3. use water, dodecylbenzenesulfonic acid solution washing precipitation substantially colourless to filtrate successively, vacuum-drying 48h at 40 DEG C, obtain the polyaniline adulterated;
(2) by film-forming resin and solidifying agent, glass flake, filler, auxiliary agent and electro-conductive material precise, drop in agitator, mix 6-15 minutes, after fully mixing, be discharged in the hopper of double-screw type forcing machine, forcing machine one district temperature 90-95 is spent, two district's temperature 100-105 are spent, and screw speed 350-450 revs/min, extrudes, cooling compressing tablet, obtains normal temperature tablet;
(3) then normal temperature tablet and nano aluminium oxide or nano fumed silica are mixed even, enter again in pulverizer and carry out micronizing, sieve, control particle size range at D50=35-50, then test following index: dry powder flow, surface resistivity, tracking index, pliability test, cathodic disbonding test, flame retardant properties test, pipe flatten coating test etc.; All qualifiedly namely obtain vertical shaft fluidized bed dipping special anti-corrosion conductive powder paint.
The application of vertical shaft fluidized bed dipping special anti-corrosion conductive powder paint as above in vertical shaft fluidized-bed dipping painting anticorrosion conductive conduits.
Advantage of the present invention and positively effect are:
1, powder coating of the present invention has high glass transition temperature, light specific gravity, general≤1.1g/cm
3, be easy to the feature of fluidisation, even if add up to a hundred tons of powder in 20 meters of deep-wells, also can fluidisation to be even easily, this is core object of the present invention, and proportion is too large, is difficult to fluidisation, just can not by the method for vertical shaft dip-coating; This powder is for hot dip coating construction technology, and coating has surface conduction characteristic and high temperature resistant poach characteristic after becoming paint film, is applicable to the anticorrosive coating of pit mining explosion-proof gas pipeline, natural gas line, the isometric linear workpiece of liquefied gas pipeline; Adapt to vertical shaft fluidized bed deep and can reach 20 meters, still have good fluidizing performance, this is that general powder is difficult to realize.
2, powder coating of the present invention contains the coating of a certain amount of polyaniline, in acid condition, there is anodic oxidation reactions, quick recovery surface passivation layer, even if corrosive deposit immerses, passivation layer can as the second barrier, also the generation of corrosion can be hindered, ensure that antiseptic property and the self-healing properties of coating, warping resistance, snappiness significantly improve, and have the characteristic of improved corrosion, scratch resistance capability; The selfreparing passive behavior of the barrier property of common coating and polyaniline combines by this powder coating, realize once getting final product thick painting, construction is simple, avoid the workpiece after coating in construction process after breakage, from the hidden danger of breaking point starting point corrosion, sticking power, the corrosion resistance of coating also have passed GB correlation detection.
3, powder coating coating of the present invention can be conducted electricity, and ensure that mine gas pipeline can be led and destatic, be against any misfortune generation.
4, the color stuffing of powder coating of the present invention not only play color matching used, also critical impact is produced on antiseptic property.Filler preferably " basalt chopped fiber powder ", basaltic major ingredient is silicon-dioxide, aluminium sesquioxide, ferric oxide, calcium oxide, magnesium oxide (also having a small amount of potassium oxide, sodium oxide), wherein dioxide-containing silica is maximum, accounts for about 40 five to five ten percent.Basaltic magma, when temperature in degree Celsius 1,200 degree, can be pumped into glass yarn, and stronger than general glass wool cloth alkali-resistivity, resistance to elevated temperatures is good, and the silk special process be then pumped into by magma is short is cut into fiber, then fiber is worn into micron powder and can use.Basalt fibre powder main performance index: density: 2.6g/cm
3, water ratio: <0.5%, Fibre diameter: 9-18 μm, length-to-diameter ratio: 4:1-8:1, breaking tenacity: >2000Mpa, use temperature :-260-1000 DEG C, flame retardant properties: limiting oxygen index(LOI) (Loi) >70, granularity: 200-600 order.This basalt fibre powder can improve anticorrosive coating coating hardness and wear resistance, coating internal stress can be effectively reduced, improve resistance to impact shock and the sticking power of coating, the second-order transition temperature of coating can also be improved, effectively can stop the process of osmosis of corrosive medium in non-corrosibility paint coatings and improve the temperature tolerance of coating, in fact basalt fibre powder is exactly the ultrashort basalt fibre cut, the distribution in 3 D stereo confusion in coating, form netted strength layer, thus strengthen the adhesion strength of coating every nook and cranny, do not ftracture not blistering
5, in the inventive method, the polymerization yield rate of the polyaniline that the explained hereafter of synthesized polyaniline obtains is greater than 80%, the specific conductivity of polyaniline is greater than 1S/cm, and, the plurality of advantages such as emulsion polymerization rate of polymerization is high, molecular weight of product is high, have good thermostability and particle size is even, the method method is simple, easy to operate, save production cost, improve the economic benefit of enterprise.
Accompanying drawing explanation
Fig. 1 is the erosion resistance of powder coating of the present invention and the Performance comparision figure of common non-invention layer, wherein: 1 (a) figure is: the coating initial state figure of one of common coating and the present invention; 1 (b) figure is: accelerated corrosion test is after 12 days, and destroying appears in common layer and coating of the present invention is fine; 1 (c) figure is: 15 days post-dryings, and good containing coating self-regeneration of the present invention, common coating cannot be repaired;
Fig. 2 is the anatomical connectivity schematic diagram of vertical shaft fluidized bed dipping device of the present invention;
Fig. 3 is the vertical view of fluidized plate and frame support bracket thereof in Fig. 2;
Fig. 4 is the upward view of Fig. 3;
Fig. 5 is the vertical view of immersed type pipe baffle grid in Fig. 2.
Embodiment
Below by specific embodiment, the invention will be further described, and following examples are descriptive, is not determinate, can not limit protection scope of the present invention with this.
The method used in the present invention if no special instructions, is ordinary method; The reagent used in the present invention if no special instructions, is conventional reagent.
The glass flake used in the present invention, can be general industry material, its major ingredient be mica, quartz sand, soft silica; Fineness 200-1000 order, it is flakey that electron microscope amplifies outward appearance, effectively can intercept the invasion of corrosive medium after film forming, and proportion is comparatively light simultaneously, is beneficial to deep-well fluidisation.Glass flake is a kind of very thin glass fragment.It is by the melten glass of more than 1000 DEG C, the glass fibre under the state of the drawing force that froths, is in, cool rapidly, broken, to mill and obtained by the step of preparation process such as screening.Adopting glass flake to make coating key character, is water-fast and the osmosis of ion significantly promotes, use as corrosion protective layer, and it also by than adopting the packing materials such as mica, Calucium Silicate powder and pure aluminium silicate, has more superior performance.It suppresses the perviousness of gas and water vapor, also depends on the characteristic of glass flake filler, comprises the size of scale, shape, packing ratio, the cohesive force of scale and resin, orientation, and the thickness etc. of coating.
The electro-conductive material used in the present invention may be: wherein one or more the mixture such as pros-and-cons type conductive acetylene black (being conductive carbon black again), conductive carbon nanotube, electrically conductive graphite, conductive mica powder, conductive metal powder, electrically conductive polyaniline, the conducting value very different of the electro-conductive material of different manufacturers, be not what kind can meet these processing condition, in every case be the scheme adopting above close thinking, coatingsurface resistance 1 × 10 can be realized by debugging
3---1 × 10
9the scheme of ohm can.Can preferred conductive material be doped conductive polyaniline.
Nano aluminium oxide used in the present invention or thermal silica be Aeroxide Alu C or Aeroxide Alu C805 or
200 or
380, purchase from Evonik Degussa Industries (German Evonik Degussa Corp.), addition is between thousandth to five, after being dry mixed, wears into ultra-micro powder together with signature sheet stock.Similar product is domestic also has production, and the product that every performance function is similar and thinking, all in the protection domain of this patent.
Film-forming resin used in the present invention and solidifying agent can be the collocation of following category:
(1) epoxy resin+phenols curing agent+imidazole and its derivants system ≈ (50-70): (12-16): (3-8);
(2) epoxy resin+polyester resin system ≈ 50:50 or 60:40 or 70:30 or 80:20;
(3) urethane+different fluorine that ketone isocyanate systems ≈ 80:20;
(4) Epocryl (GMA derivative or multipolymer)+long chain dicarboxylic acid system ≈ 80-83:17-20;
(5) epoxy resin+polyamine+imidazole and its derivants system;
(6) thermoplastic resin system, as PE, PP, PVDF etc.;
Above-mentioned epoxy resin comprises the solid epoxy of E-12 type, E-10 type and other models that single stage method and two-step approach are produced, and comprises that solvent method and WATER-WASHING METHOD are produced and modification or derivative goods.
The auxiliary agent used in the present invention is mixture, and major ingredient is: (1) butyl polyacrylate flow agent BYK361N, from BYK Additives and Instruments (German Bi Ke auxiliary agent and instrument company); (2) brightening agent BLC701B (South Sea, Ningbo chemistry), (3) defoamer Ceraflour 961; Ceraflour962 is from BYK Additives and Instruments (German Bi Ke auxiliary agent and instrument company) or st-yrax (purchased from chemical industry green wood company large in Jiangxi's rise), and its parts by weight are as follows:
Flow agent: 16 ~ 22 parts;
Brightening agent: 10 ~ 20 parts;
Defoamer: 4 ~ 8 parts.
Embodiment 1
The preparation method of vertical shaft fluidized bed dipping special anti-corrosion conductive powder paint and an application, its raw material forms component and parts by weight are respectively:
The step of the preparation method of above-mentioned vertical shaft fluidized bed dipping special anti-corrosion conductive powder paint is as follows:
(1) the preparation of polyaniline:
1. emulsion polymerization synthesized polyaniline technique: add aniline and dodecylbenzene (ratio of the amount of substance of the two is 2:1) in the reactor, add water after mixing successively, (two is all solvent to dimethylbenzene, do not participate in reaction, appropriate), abundant stirring, to obtaining transparent emulsion;
2. then in transparent emulsion, ammonium persulphate (NH is dripped
4)
2s
2o
8the aqueous solution (ammonium persulphate is 1:1 with the ratio of the amount of aniline), system color slowly deepens, keep system temperature 0 ~ 20 DEG C, continue stirring 30 minutes, after during static storing 24, then add proper amount of acetone breakdown of emulsion (add-on is 5% ~ 20% of overall solution volume in reactor), with appropriate ethanol or acetone (add-on is 1 ~ 10 times of overall solution volume) repetitive scrubbing 3 ~ 4 times, remove ethanol or acetone, filter to obtain precipitation;
3. use water, dodecylbenzenesulfonic acid solution washing precipitation substantially colourless to filtrate successively, vacuum-drying 48h at 40 DEG C, obtain the polyaniline powder adulterated; The molecular structural formula of preparation-obtained polyaniline is:
(2) the preparation of powder coating:
By step (1) in the polyaniline powder of synthesis and film-forming resin and solidifying agent, auxiliary agent, color stuffing is pressed formula rate and is weighed accurately, drop in agitator, mix 6-15 minutes, after fully mixing, be discharged in the hopper of double-screw type forcing machine, forcing machine one district temperature 90-95 is spent, two district's temperature 100-105 are spent, screw speed 350-450 revs/min, extrude, cooling compressing tablet, then normal temperature tablet and nano aluminium oxide or white carbon black are mixed even, enter again in ACM air classifying Cyclonic pulverizer and carry out micronizing, sieve, control particle diameter D50 ≈ 35-50, laser particle analyzer can be adopted to test granularity, then following index is tested: dry powder flow, surface resistivity, tracking index, pliability test, cathodic disbonding is tested, flame retardant properties is tested, pipe flattens coating test etc., all qualifiedly be vertical shaft fluidized bed dipping special anti-corrosion conductive powder paint product.
Pipeline after application need send third party to detect certification and could apply in engineering, and national unique authentication mechanism is coating fire-resistant antistatic institute of Shanghai Coal Mining Research Institute of former the Ministry of Coal Industry (in south bridge town, Spring in Pig House of Shanghai Fengxian district); Also need the detection certification by Beijing Safe Production Supervision office of Mei Ke institute simultaneously.
Embodiment 2
The preparation method of vertical shaft fluidized bed dipping special anti-corrosion conductive powder paint and an application, its raw material forms component and parts by weight are respectively:
The preparation method of above-mentioned vertical shaft fluidized bed dipping special anti-corrosion conductive powder paint, step is as follows:
The each composition of precise, drop in agitator, mix 6-15 minutes, after fully mixing, be discharged in the hopper of double-screw type forcing machine, forcing machine one district temperature 90-95 is spent, two district's temperature 100-105 are spent, screw speed 350-450 revs/min, extrude, cooling compressing tablet, then normal temperature tablet and nano aluminium oxide or white carbon black are mixed even, enter again in ACM air classifying Cyclonic pulverizer and carry out micronizing, sieve, control particle diameter, with laser particle analyzer test granularity D50 ≈ 35-50, then following index is tested: dry powder flow, surface resistivity, tracking index, pliability test, cathodic disbonding is tested, flame retardant properties is tested, pipe flattens coating test etc., all qualifiedly be vertical shaft fluidized bed dipping special anti-corrosion conductive powder paint product.
Pipeline after application need send third party to detect certification and could apply in engineering, and national unique authentication mechanism is coating fire-resistant antistatic institute of Shanghai Coal Mining Research Institute of former the Ministry of Coal Industry (in south bridge town, Spring in Pig House of Shanghai Fengxian district); Also need the detection certification by Beijing Safe Production Supervision office of Mei Ke institute simultaneously.
Embodiment 3
The preparation method of vertical shaft fluidized bed dipping special anti-corrosion conductive powder paint and an application, its raw material forms component and parts by weight are respectively:
Nano aluminium oxide or nano fumed silica (being commonly called as white carbon black): 1 ~ 5kg.
The preparation method of above-mentioned vertical shaft fluidized bed dipping special anti-corrosion conductive powder paint is with embodiment 1.
Embodiment 4
The preparation method of vertical shaft fluidized bed dipping special anti-corrosion conductive powder paint and an application, its raw material forms component and parts by weight are respectively:
The preparation method of above-mentioned vertical shaft fluidized bed dipping special anti-corrosion conductive powder paint is with embodiment 1.
The practical application effect of powder coating of the present invention and test situation:
In acidic medium, there is the carbon steel of polyaniline rete than there is no the solidity to corrosion of rete and exceed 100 times; And be in the medium of 7 in pH value, there is the carbon steel of polyaniline rete only to exceed 2 times than the solidity to corrosion of reduction-state; In the seawater of pH value 8.0 ~ 9.4, not evidence suggests that polyaniline has good antiseptic property.This structure that can be interpreted as polyaniline is relevant with pH value.So experiment conclusion shows, polyaniline coating only just can put out the antiseptic property of its excellence to good use in sour environment, and in alkaline environment, mainly also by glass flake and basalt chopped fiber powder and resin coating.Conductivity then mainly provides by polyaniline and graphitized carbon black.
By different application modes and analysis test method (such as, in ASTM to the examination criteria method of coating; Electrochemical test method measures open circuit potential, corrosion potential, corrosion current and polarization impedance etc.; The structure of the methods analyst matallic surface layers such as XPS and SEM and chemical composition) have studied polyaniline paint to the anticorrosion ability of metal (mainly ferrous metals) and anticorrosion mechanism, (relevant test data is shown in a, b, c in accompanying drawing 3 to the experimental results.) demonstrate the antiseptic property of powder coating of the present invention compared with conventional protective system, there is significant raising.
The erosion resistance of coating of the present invention and the Performance comparision of common non-invention layer, wherein:
1 (a) figure is: the coating initial state of one of common coating and the present invention;
1 (b) figure is: accelerated corrosion test is after 12 days, and destroying appears in common layer and coating of the present invention is fine;
1 (c) figure is: 15 days post-dryings, and good containing coating self-regeneration of the present invention, common coating cannot be repaired.
Note: (Original in diagram: the original state of testing plate; SI: testing plate is through 12% salt solution, and 75 DEG C are soaked the states after 290 hours; Ov: testing plate is through the state of 80 DEG C of bakings after 72 hours); (low frequency, the preservative effect of the higher coating of resistance when namely X-coordinate is-1 is better).
Implement the vertical shaft fluidized bed dipping device of the preparation method of vertical shaft fluidized bed dipping special anti-corrosion conductive powder paint as above, as shown in Figure 2, described device comprises vertical shaft 4, fluidized-bed inner bag 5, fluidized plate and frame support bracket 8 thereof, air compression plant and gas storage surge tank 9 and immersed type pipe baffle grid 6, described vertical shaft is the hollow form arranged downwards from ground level 3, described fluidized-bed inner bag is coaxially movably placed in this vertical shaft, because activity is installed, therefore this fluidized-bed inner bag can take out from this vertical shaft, this fluidized-bed inner bag is open top, the hollow form of sealed bottom, treat that dip-coating pipeline is vertically placed in this fluidized-bed inner bag, carry out dip-coating wherein, bottom in this fluidized-bed inner bag arranges air compression plant and gas storage surge tank, in fluidized-bed inner bag above this air compression plant and gas storage surge tank, fluidized plate and frame support bracket thereof are coaxially set, in fluidized-bed inner bag above this fluidized plate and frame support bracket thereof, immersed type pipe baffle grid are coaxially set.
As shown in Figure 3 and Figure 4, described fluidized plate and frame support bracket comprise fluidized plate 10 and frame support bracket 12, described frame support bracket is coaxially installed on fluidized-bed inner bag, this resting support can bear tens of tons of powder coating or molding powder on it, be close to above this frame support bracket and fluidized plate is set, this fluidized plate is coaxially installed on fluidized-bed inner bag and its periphery and fluidized-bed inner bag are tightly connected, thus can not leak gas from surrounding, in this fluidized plate vertically, along the circumferential direction uniform interval several micropore 11 is set.In the present embodiment, the diameter of described micropore is 20-200 microns, pressurized air in air compression plant and gas storage surge tank from bottom to top can enter the fluidized bed space of fluidized-bed inner bag middle and upper part through micropore, by fluidized plate and frame support bracket, fluidized-bed inner bag is separated into upper and lower two parts like this, just a space is formed below resting support, this space is " air chamber ", and namely air compression plant and gas storage surge tank are arranged at institute indoor.
As shown in Figure 5, described immersed type pipe baffle grid comprise multiple parallel, spaced parallel cylindrical tube layer 13, described parallel cylindrical tube layer comprises multiple parallel, spaced pipe 7, the two ends of this pipe are installed on the inwall of fluidized-bed inner bag, and these every two adjacent parallel cylindrical tube layer are that right-angled intersection is solidly installed.These immersed type pipe baffle grid mainly eliminate bubble, prevent bubble gather increase and final surface " dirt is quick-fried ", to make in vertical shaft powder coating or molding powder fluid density evenly, play homogeneously fluidized bed, eliminate the effect of bubble " implosion " phenomenon, improve coating quality, also can prevent top junk from smashing microwell plate simultaneously.In the present embodiment, described parallel cylindrical tube layer is 3-5 layers, and every interlamellar spacing is 20-30 centimetres; Described pipe diameter is 80-100 millimeters, parallel distance is 15-30 centimetres between pipe; Described immersed type pipe baffle grid are arranged at 0.5-1.5 meters of above fluidized plate.
In the present embodiment, described vertical shaft, for dig a bite deep-well downwards from ground level, forms vertical shaft outer wall with masonry or concrete structure brick work, and vertical shaft puzzles and generally does waterproof, antifreeze, rotproofing afterwards, so that durable in use, inside can not produce ponding.Well depth with reference to the length setting being coated workpiece, slightly deeply a bit, generally can will be deeper than Workpiece length about 1 meter, the diameter of vertical shaft is determined according to the diameter of coated article, be greater than diameter of work, common vertical shaft significant depth is generally at 6-20 meters, and effective diameter is generally between 0.5-3.0 meters.Vertical shaft is dark below ground 6-20 meters, can reduce the requirement to factory building height like this, because steel pipe will vertically soak down and lift, has particular requirement to factory building height.
In the present embodiment, described fluidized-bed inner bag is welded by stainless-steel roll, also can roll up weldering by steel plate or other pressure tight metal materials or non-metallic material and form, then carry out rotproofing.The degree of depth and " vertical shaft " outer wall etc. are dark, also can slightly be shorter than " outer wall ".Inner bag can hang out vertical shaft with the need, to clear up colour changing and maintenance.The top 2 of this fluidized-bed inner bag is above the ground level, such as be 20-40 centimetres, the transverse width on top wider than the transverse width below fluidized-bed inner bag, will be shaped with powder coating overflow port 1 in the side, top of fluidized-bed inner bag, and unnecessary coating can be recycled thus in the overflow of powder coating overflow port.
In the present embodiment, described air compression plant and gas storage surge tank comprise air compression plant and gas storage surge tank, described air compression plant is Root's blower, the general 0.04-0.4MPa of blast of this Root's blower, and this blower fan generally can provide higher air quantity and suitable blast; Described gas storage surge tank can cushion the pressurized air of 5-50 cubic metres, plays a part smooth air flow and clean air.
In the present embodiment, described device also comprises heating installation and hanging device, described heating installation is baking oven or medium-frequency heating coil, described hanging device is upending frame, steel turntable or driving, this heating installation is used for heating by coated article (steel pipe or section bar), and this hanging device is used for slinging in vertical shaft device to by coated article (steel pipe or section bar).Employing baking oven heats, and efficiency is lower, and heating a pipeline about needs 30-120 minutes; Adopt medium-frequency heating coil, power is large, but efficiency is high, environment-friendly, sanitary and energy-saving, and equipment volume is little does not account for hall space, and several tons heavy tens meters of long steel pipes can be heated to 120 DEG C by tens seconds--and 160 DEG C.Hanging device can according to the convenient design of mill construction, and with upending frame or driving, can be not construed as limiting, both utility appliance all can be regarded as in the conventional equipment in this area, is not therefore described in detail, and is just briefly described.
The production operation method of this vertical shaft fluidized bed dipping device is as follows:
1, coated article (steel pipe or section bar) is done the surface treatments such as degreasing and rust removal, the ordinary method that the industries such as phosphatization, sandblasting, ball blast allow can be adopted.Detailed pre-treatment regulation is generally had in country or industry standard.
2, steel pipe is heated to 120 DEG C--and 160 DEG C.Baking oven heating or heating in medium frequency.
3, molding powder or powder coating are poured in vertical shaft inner bag reach about 60% of shaft depths.
4, open the compressed air control valve of air compression plant, regulate air-flow, powder starts floating fluidized, as the water of flowing, till bisque rises to overflow port; If deficiency need supplement powder.
5, to try fluidized state with examination pole, examination pole freely can fall non-resistance, just proves that fluidisation is excellent.
6, the workpiece hoist cable heated and fixture etc. are sling, in quick immersion vertical shaft, till submergence, powder melted by heat adhere on tube wall around tube wall, is risen from well head by Quick after 4-7 seconds after steel pipe immerses, namely application completes, and so go round and begin again production.
7, as reheated, enter baking oven second-heating again after can setting level, if do not need to reheat, set level the solidification of rear waste heat, after cooling, namely painting work finishes.
8, after fluidized bed powder consumes in production process, if bed is high not enough, regularly powder need be mended, and so forth.
The technical parameter of the present embodiment device:
Model specification: SYD--2015;
Be suitable for material: powder coating or molding powder;
Vertical shaft capacity: 6--150 cubic meter;
Dip-coating speed: 4 ~ 7 seconds/root;
Power supply: 380V/50HZ;
Resting support height: 7-25 meters;
Temperature range: 120 ~ 160 DEG C.
This device is applicable to dip-coating natural gas line, fire protection pipeline, fiery mine pipeline, petroleum pipe line, aluminium alloy extrusions, steel I-beam, drinking water pipeline etc.Can realize fast, application in enormous quantities, production efficiency is fast doubly a lot of compared with electrostatic spraying, and can realize disposable thick painting and can reach Standard.
The one application of powder coating of the present invention can be as follows:
1, powder coating of the present invention is poured in the inner bag of vertical shaft fluidized bed plant, reach about 60% of shaft depths
2, open compressed air control valve, regulate air-flow, powder starts floating fluidized, till bisque rises to overflow port; If deficiency need supplement powder;
3, to try fluidized state with examination pole, examination pole freely can fall non-resistance, just proves that fluidisation is excellent;
4, coated article (steel pipe or section bar) is done the surface treatments such as degreasing and rust removal, the ordinary method that the industries such as phosphatization, sandblasting, ball blast allow can be adopted.Detailed pre-treatment regulation is generally had in country or industry standard.
5, steel pipe is heated to 120 DEG C--and 160 DEG C.Baking oven heating or heating in medium frequency.
6, the workpiece hoist cable heated and fixture are sling, immerse in vertical shaft, till submergence fast; Mention after 4-7 seconds;
7, as reheated, enter baking oven second-heating again after can setting level, if do not need to reheat, set level the solidification of rear waste heat, after cooling, namely painting work finishes.
8, after fluidized bed powder consumes in production process, if bed is high not enough, regularly powder need be mended, and so forth.
Powder coating of the present invention is applied by domestic large-scale pipeline manufacturing enterprise, as Qufu City, Shandong Province east grand Guan Ye, Dalian Shi Wang pipeline corrosion protection company etc.Be coated with tubing and sent in western gas east engineering, Jin Mei group, state to throw in the mining engineering such as Xin Ji colliery and widely apply.
Claims (10)
1. a vertical shaft fluidized bed dipping special anti-corrosion conductive powder paint, is characterized in that: its raw material forms component and parts by weight are:
2. vertical shaft fluidized bed dipping special anti-corrosion conductive powder paint according to claim 1, is characterized in that: its raw material forms component and parts by weight are:
3. vertical shaft fluidized bed dipping special anti-corrosion conductive powder paint according to claim 1 and 2, is characterized in that: described film-forming resin and solidifying agent are the one in the collocation of following category:
(1) epoxy resin+phenols curing agent+imidazole and its derivants system, mass ratio is (50-70): (12-16): (3-8);
(2) epoxy resin+polyester resin system, mass ratio is 50:50 or 60:40 or 70:30 or 80:20;
(3) urethane+different fluorine that ketone isocyanate systems, mass ratio is 80:20;
(4) Epocryl+long chain dicarboxylic acid system, mass ratio is 80-83:17-20;
(5) epoxy resin+polyamine+imidazole and its derivants system;
(6) thermoplastic resin system.
4. vertical shaft fluidized bed dipping special anti-corrosion conductive powder paint according to claim 1 and 2, is characterized in that: the fineness of described glass flake is 200-1000 order; Or described filler is one or more mixtures in process white, ultra-fine barium sulfate, activared carbon sulfur barium, basalt chopped fiber powder, silicon-dioxide, wollastonite powder, silicon powder, mica powder, sericite.
5. vertical shaft fluidized bed dipping special anti-corrosion conductive powder paint according to claim 1 and 2, it is characterized in that: described auxiliary agent is mixture, its composition and parts by weight are:
Butyl polyacrylate flow agent: 16 ~ 22 parts;
Brightening agent: 10 ~ 20 parts;
Defoamer or st-yrax: 4 ~ 8 parts;
Be mixed into a kind of raw material in this ratio, and then press formula rate weighing use.
6. vertical shaft fluidized bed dipping special anti-corrosion conductive powder paint according to claim 1, is characterized in that: described electro-conductive material is for can realize coatingsurface resistance 1 × 10
3---1 × 10
9the electro-conductive material of ohm.
7. vertical shaft fluidized bed dipping special anti-corrosion conductive powder paint according to claim 6, is characterized in that: described electro-conductive material is one or more mixture in conductive carbon black, conductive carbon nanotube, electrically conductive graphite, conductive mica powder, conductive metal powder, electrically conductive polyaniline.
8. the preparation method of the vertical shaft fluidized bed dipping special anti-corrosion conductive powder paint as described in any one of claim 1 to 7, is characterized in that: step is as follows:
By film-forming resin and solidifying agent, glass flake, filler, auxiliary agent and electro-conductive material precise, drop in agitator, mix 6-15 minutes, after fully mixing, be discharged in the hopper of double-screw type forcing machine, forcing machine one district temperature 90-95 is spent, two district's temperature 100-105 are spent, and screw speed 350-450 revs/min, extrudes, cooling compressing tablet, obtains normal temperature tablet;
Then normal temperature tablet and nano aluminium oxide or nano fumed silica are mixed even, enter again in pulverizer and carry out micronizing, sieve, control particle size range at D50=35-50, then test following index: dry powder flow, surface resistivity, tracking index, pliability test, cathodic disbonding test, flame retardant properties test, pipe flatten coating test etc.; All qualifiedly namely obtain vertical shaft fluidized bed dipping special anti-corrosion conductive powder paint.
9. the preparation method of vertical shaft fluidized bed dipping special anti-corrosion conductive powder paint according to claim 8, is characterized in that: step is as follows:
(1) described electro-conductive material is polyaniline, and its preparation process is as follows:
1. emulsion polymerization synthesized polyaniline technique: add in the reactor in aniline: the ratio of the amount of substance of dodecylbenzene is that the ratio of 2:1 is for adding aniline and dodecylbenzene, water, dimethylbenzene is added successively after mixing, abundant stirring, to obtaining transparent emulsion;
2. then in transparent emulsion in ammonium persulphate: the ratio of the amount of substance of aniline is that the ratio of 1:1 drips ammonium persulphate (NH
4)
2s
2o
8the aqueous solution, system color slowly deepens, and keeps system temperature 0 ~ 20 DEG C, continues stirring 30 minutes, after during static storing 24, then adds acetone breakdown of emulsion, with ethanol or acetone repetitive scrubbing 3 ~ 4 times, removes ethanol or acetone, filters and to obtain precipitation;
3. use water, dodecylbenzenesulfonic acid solution washing precipitation substantially colourless to filtrate successively, vacuum-drying 48h at 40 DEG C, obtain the polyaniline adulterated;
(2) by film-forming resin and solidifying agent, glass flake, filler, auxiliary agent and electro-conductive material precise, drop in agitator, mix 6-15 minutes, after fully mixing, be discharged in the hopper of double-screw type forcing machine, forcing machine one district temperature 90-95 is spent, two district's temperature 100-105 are spent, and screw speed 350-450 revs/min, extrudes, cooling compressing tablet, obtains normal temperature tablet;
(3) then normal temperature tablet and nano aluminium oxide or nano fumed silica are mixed even, enter again in pulverizer and carry out micronizing, sieve, control particle size range at D50=35-50, then test following index: dry powder flow, surface resistivity, tracking index, pliability test, cathodic disbonding test, flame retardant properties test, pipe flatten coating test etc.; All qualifiedly namely obtain vertical shaft fluidized bed dipping special anti-corrosion conductive powder paint.
10. the application of vertical shaft fluidized bed dipping special anti-corrosion conductive powder paint in vertical shaft fluidized-bed dipping painting anticorrosion conductive conduits as described in any one of claim 1 to 7.
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