CN102417779B - Preparation process of bicomponent castor oil polyurethane waterproof coating - Google Patents
Preparation process of bicomponent castor oil polyurethane waterproof coating Download PDFInfo
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Abstract
A preparation process of a bicomponent castor oil polyurethane waterproof coating is characterized in that the coating is obtained by interpenetrating a component A of polyurethane prepolymer and a component B of a colorful color paste system under the action of an initiator and a catalyst; wherein the component A is obtained by allowing castor oil and 2,4-toluene diisocyanate to react in an organic solvent dissolved with an initiator; the component B is obtained by mixing a blending agent, a solid pigment and/or a solid filler with a coupling agent, milling, orderly adding a alkene monomer, a catalyst, a polymerization inhibitor, and a light stabilizer, and stirring uniformly. The coating of the invention has excellent waterproofness, a good apparent state, abundant colors, good decorative effect, adjustable curing time, adjustable film flexibility and hardness, and simple operations.
Description
Technical field
The present invention relates to a kind of preparation technology of polyurethane water-proof paint
,Especially
BeThe preparation technology of two-pack Viscotrol C polyurethane water-proof paint.
Background technology
Urethane (PU-Polyurethane) is the abbreviation of polyurethane(s), and it is a kind of high molecular polymer.It is the polymkeric substance of being made by raw materials such as chainextenders such as polyisocyanates and polyether glycol or polyester polyol or small molecules polyvalent alcohol, polyamine or water or linking agents.By changing raw material type and composition, can change product form and performance thereof significantly, obtain from softness to hard the finished product.Urethane is with respect to other high-molecular coating, and it has lot of advantages, and as the material good mechanical property, the performance adjustable extent is wide, building-up properties is good etc.PU is one of synthetic paint of the world's six great development.With regard to it used range, it had jumped and has been the first place of all kinds of synthetic paint.
(Interpenetrating polymer network IPN) is the interleaving network that is run through mutually by two or more polymkeric substance to interpenetrating net polymer.The concept of interpenetrating net polymer is the Mmllar sixties
[18]Put forward, it is that method with chemistry runs through two or more polymkeric substance mutually and forms the novel complex phase polymer coating of a netted class that interweaves
[19]High-polymer molecular runs through mutually and forms the network system, between the polymkeric substance of participation IPN chemical reaction does not take place, permeates but intersect mutually, and mechanical interlocking plays " force and dissolve each other " and " synergy ".This internetwork entanglement has improved dispersiveness, the interface wetting ability of system significantly, thereby has improved relative stability, has realized the polymer performance complementation, reaches the purpose of modification.
Interpenetrating net polymer is polymer blending and compound important means, can regard a kind of innovative techniques that chemically realizes the polymer physics blend as, and IPN is one of the main developing direction of multiphase polymer in modern age.The maximum characteristics of IPN are to have adopted special preparation method, ideally with two kinds not the polymkeric substance of phase mixing intert mutually by network, entangled to each other, force compatible.And original copolymer had both had memory capability, did not lose primary characteristic; Have synergy again, a little less than strong benefit, even obtain the incomparable excellent properties of other polymkeric substance.So to the research and development of IPN coating, countries in the world are all rather paid attention to.In paint field, the application prospect of IPN is encouraging, and by the selection of raw material, the adjustment of formulating of recipe and the change of synthesis technique can make the many kinds with specified property, multiduty IPN, is used for the various new exclusive coating of preparation.Have this to close the work of this respect, also be in initial stage at present, the IPN that is used for coating mostly is synchronous IPN (SIN) and latex IPN (LIPN).When two kinds of polymer formation IPN, can improve their compatibility, widen the scope of corresponding glass transition temperature.Along with the increase of two kinds of polymeric constituent compatibilities, two second-order transition temperatures of IPN mutually near and form a broad glass transition zone, the damping of can effectively shaking in this zone, so IPN has excellent damping capacity.The application of IPN compound damping paint and noise deadener more comes benefit extensive, usually it is divided into polymer coated two kinds of extended pattern damping coating and constraint.Adopt gradation type IPN can make stretching, extension damping layer and bond course be combined into same integral body.For example: the gradation type IPN with hard surface (playing bond course) and viscoelastic internal layer (damping layer) of people such as Sperling preparation make it that fabulous damping damping capacity be arranged, so the IPN damping paint has prospect very widely.
Present polyurethane interpenetrating network type coating is many to obtain prepolymer by polyvalent alcohol and polyisocyanates reaction, and again with other synthetic resins copolymerization, remaining isocyano forms the urethane network through the moisture absorption and solidifies in the last system.Because behind the surface cure, water is hindered to the inner diffusion of filming, the moisture absorption curing ratio of the feasible inner residue isocyano of filming is difficulty, and it is long that system is done solid work the time.In addition, be difficult for discharging because the inner moisture absorption of filming is solidified the bubble that produces, make film be coated with apparent being not in good state, also influence film simultaneously and be coated with sticking power to base material.The natural renewable resource of some blending agentss, good fluidity, wettability are strong, can serve as wetting dispersing agent and crosslinking and curing agent in the polyurethane coating.Vinyl monomer such as vinylbenzene are used for the exposed conveying appliance waterproof paint can make filmed excellent abrasive and hardness, and can shorten the surface drying of filming and do solid work the time; Methyl methacrylate, butyl methacrylate, vinylformic acid, methacrylic acid are used for the exposed conveying appliance waterproof paint can make film good gloss retention, weather-proof erosion resistance and snappiness.
Summary of the invention
The object of the present invention is to provide a kind of preparation technology of two-pack Viscotrol C polyurethane water-proof paint, it can overcome the deficiency of prior art, and has excellent performance, apparent state is good, rich color, good decorating effect, and set time is adjustable, the gentle hardness of filming is adjustable, easy and simple to handle.
The technical scheme that realizes the object of the invention is: a kind of preparation technology of two-pack Viscotrol C polyurethane water-proof paint is characterized in that: be that component A and colored mill base system are that B component IPN under the effect of initiator and catalyzer obtains by base polyurethane prepolymer for use as; Wherein component A is obtained molten the reaction in the organic solvent of initiator by Viscotrol C and 2,4 toluene diisocyanate; B component is mixed with coupling agent to mill by blending agents and solid pigment and/or solid packing and is added vinyl monomer, catalyzer, stopper, photostabilizer more successively and stir and obtain.
And, comprise the steps:
(1) raw material is handled: decompression dehydration obtained in 1～2 hour under 100～120 ℃ of blending agentss, the 0.08MPa vacuum tightness; Solid pigment and/or solid packing are dried under 120 ℃ temperature and were obtained in two hours;
(2) solid pigment that blending agents and toning are needed or solid packing mix with coupling agent and are milled to suitable fineness, add vinyl monomer, catalyzer, stopper, photostabilizer stirring again and successively and obtain uniform and stable B component;
(3) earlier with molten organic solvent and 2 with initiator, the 4-tolylene diisocyanate adds the Viscotrol C that in batches adds again in the reactor after the vacuum hydro-extraction, be not more than in water or air cycle condensation and in temperature control under 50 ℃ the condition and reacted 1 ~ 3 hour, stirring obtains component A;
(4) component A and B component are mixed by weight 1:0.5 ~ 4, add an amount of organic solvent again and be adjusted to appropriate viscosity, stir, left standstill 10-60 minute, and brushed under the room temperature or be sprayed on to solidify on the different base materials and obtained colored exposed conveying appliance interpenetrating(polymer)networks two-pack Viscotrol C polyurethane water-proof paint in 30 minutes ~ 8 hours.
And the used blending agents of step (1) is 1 ~ 5 kind in glycerine, glycol ether, tetramethylolmethane, sorbyl alcohol, the TriMethylolPropane(TMP); The used solid pigment of step (1) is 1 ~ 10 kind in titanium dioxide, red iron oxide, carbon black, zinc oxide, zinc sulfide white, medium chrome yellow medium yellow, phthalocyanine blue, phthalocyanine green, ultramarine, the toluidine red; Solid packing is that blue or green cream powder, granularity are 1 ~ 5 kind in 600-800 purpose light calcium carbonate, wilkinite, talcum powder, the barite; The used vinyl monomer of step (2) is 1～6 kind in vinylbenzene, methyl methacrylate, butyl methacrylate, vinyl cyanide, the acrylic or methacrylic acid; Coupling agent is titanate coupling agent; Catalyzer is 1～4 kind in dibutyl tin dilaurate, stannous octoate, triethylamine, the triethylene diamine; Stopper is Resorcinol; Photostabilizer is oxidation inhibitor four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol ester (1010), Octabenzone (UV-531), 2-(2-hydroxyl-3,5-two fourth uncles base phenyl)-5-chlorinated benzotriazole (UV-327), 2-(2 '-hydroxyl-3 ', 5 '-the diamyl phenyl) benzotriazole (UV-328), 2-hydroxyl 4-1～5 kind in the octyloxy benzophenone (UV-292).Wherein, 1010, UV-531, UV-327, UV-328, UV-292 are respectively its commodity popular name; The used initiator of step (3) is benzoyl peroxide or Diisopropyl azodicarboxylate; Organic solvent is 1～6 kind in toluene, dimethylbenzene, ethyl acetate, butylacetate, acetone, the methylethylketone.
And component A and B component weight ratio are 1:0.5 ~ 4; In component A, by weight percentage, the Viscotrol C consumption is 30% ~ 75%, and the 2,4 toluene diisocyanate consumption is 15% ~ 60%, and consumption of organic solvent is 5% ~ 25%, and initiator amount is 0.2 ~ 2%; In B component, by weight percentage, the blending agents consumption is 10% ~ 30%, solid pigment or solid packing consumption are 20% ~ 45%, and the vinyl monomer consumption is 20 ~ 55%, and the coupling agent consumption is 0.05 ~ 1%, catalyst levels is 0.05 ~ 1%, and the stopper consumption is 0.05 ~ 1%, and the photostabilizer consumption is 0.05 ~ 2%.
The present invention utilizes blending agents, vinyl monomer as linking agent, make cross-linking system contain simultaneously with two keys and hydroxyl, this cross-linking system can either utilize the two keys in its pair key and the base polyurethane prepolymer for use as to carry out copolymerization or self-polymeric reaction forms the polyolefine network, can utilize remaining isocyano reaction formation urethane network in its hydroxyl and the base polyurethane prepolymer for use as again, make curing reaction not rely on moisture and finish.Simultaneously, use blending agents to make linking agent, enlarged the cross-linker molecules chain, improved the low temperature flexibility of filming, vinyl monomer is made linking agent and can be improved the apparent condition of filming and regulate coating performance.Processing unit of the present invention is simple, and is easy to operate, is conducive to industrial mass production; The colored interpenetrating(polymer)networks two-pack of the exposed conveying appliance that obtains Viscotrol C polyurethane water-proof paint has excellent water resistance, better mechanical property, ageing-resistant performance, resistance to chemical corrosion, and rich color, good decorating effect, not only can use at the exposed parts of buildings, play waterproof and decoration function simultaneously, but also can use at non-exposed parts, have price and environment-friendly advantage, product can be at the top-grade building thing, highway, bridge, high-speed railway, the drome, product such as large stadium uses, comparatively wide applications is arranged, have fine economic and social benefit.
Description of drawings
Fig. 1 is thermogravimetric and the heat flow curve figure after two-pack Viscotrol C polyurethane water-proof paint varnish solidifies.
Wherein curve a is the thermogravimetric curve after colored exposed conveying appliance interpenetrating(polymer)networks two-pack Viscotrol C polyurethane water-proof paint varnish solidifies, and b is the heat flow curve after colored exposed conveying appliance interpenetrating(polymer)networks two-pack Viscotrol C polyurethane water-proof paint varnish solidifies.
Through test, compositional range involved in the present invention all can realize goal of the invention, is described in further detail by the following examples:
A is the thermogravimetric curve figure after colored exposed conveying appliance interpenetrating(polymer)networks two-pack Viscotrol C polyurethane water-proof paint varnish solidifies in the accompanying drawing 1, has three steps weightless; B is the heat flow curve figure after the colored interpenetrating(polymer)networks two-pack of exposed conveying appliance Viscotrol C polyurethane water-proof paint varnish solidifies, and three endotherm(ic)peaks are arranged.Illustrate that the degraded of the colored interpenetrating(polymer)networks two-pack of exposed conveying appliance Viscotrol C polyurethane water-proof paint varnish divides three ones and carries out.This is because exist two kinds of cross-linked networks in this is filmed: the polyolefine network of the free-radical polymerized formation of two keys process in contained pair of key of Viscotrol C and the vinyl monomer in the performed polymer; In residue-NCO in the performed polymer and the colored mill base system in the Viscotrol C-OH forms the urethane network.Physics windings by molecular chain of two kinds of networks, hydrogen bond etc. are in conjunction with the stable IPN system of formation.
Embodiment one:
White exposed conveying appliance waterproof paint: concrete proportioning is: component A: Viscotrol C 20.0%, 2,4 toluene diisocyanate 38.07%, dimethylbenzene 8.6%, Diisopropyl azodicarboxylate 0.2%; Component B: glycol ether 8.0.%, titanium dioxide 15.5%, talcum powder 2.0%, ultramarine 0.05%, coupling agent YB-201A (can adopt the titanate coupling agent of Changzhou Ya Bangya space auxiliary agent company limited) 0.08%, methacrylic acid formic acid 7.0%, antioxidant 1010 0.1%, UV-292 0.1%, Resorcinol 0.1%, stannous octoate 0.1%, triethylene diamine 0.1%.Component A and component B are mixed, add proper amount of diluting, stir, left standstill 30 minutes, be cast on the glass template under the room temperature and be sprayed on the steel plate, 30 ℃ of following constant temperature 7 days.Coating surface drying time on the glass template is 2 hours, and the coating surface drying time on the steel plate is 2 hours; Coating gloss 60.3 on the steel plate, hardness 3H; It is 10.75MPa that filming on the glass template measured its tensile strength according to national polyurethane water-proof paint standard at XLD-3 type electronic tensile test machine, and elongation at break is 275%; The electronic waterproof determinator of LTD-A type is measured its watertightness, and 0.4MPa30min is waterproof.
Embodiment two:
White exposed conveying appliance waterproof paint: concrete proportioning is: component A: Viscotrol C 30.07%, 2,4 toluene diisocyanate 20.0%, dimethylbenzene 8.6%, Diisopropyl azodicarboxylate 0.2%; Component B: glycol ether 8.0.%, titanium dioxide 15.5%, talcum powder 2.0%, ultramarine 0.05%, coupling agent YB-201A (can adopt the titanate coupling agent of Changzhou Ya Bangya space auxiliary agent company limited) 0.08%, methacrylic acid formic acid 7.0%, antioxidant 1010 0.1%, UV-292 0.1%, Resorcinol 0.1%, stannous octoate 0.1%, triethylene diamine 0.1%.Component A and component B are mixed, add proper amount of diluting, stir, left standstill 30 minutes, be cast on the glass template under the room temperature and be sprayed on the steel plate, 30 ℃ of following constant temperature 7 days.Coating surface drying time on the glass template is 3 hours, and the coating surface drying time on the steel plate is 2 hours; Coating gloss 60.4 on the steel plate, hardness 3H; It is 8.65MPa that filming on the glass template measured its tensile strength according to national polyurethane water-proof paint standard at XLD-3 type electronic tensile test machine, and elongation at break is 363%; The electronic waterproof determinator of LTD-A type is measured its watertightness, and 0.4MPa30min is waterproof.
Embodiment three:
White exposed conveying appliance waterproof paint: concrete proportioning is: component A: Viscotrol C 27.0%, 2,4 toluene diisocyanate 14.85%, dimethylbenzene 4.2%, ethyl acetate 2.1%, Diisopropyl azodicarboxylate 0.3%; Component B: glycol ether 8.5%, titanium dioxide 16.5%, talcum powder 3.0%, ultramarine 0.15%, coupling agent YB-201A (can adopt the titanate coupling agent of Changzhou Ya Bangya space auxiliary agent company limited) 0.5%, methacrylic acid formic acid 21.8%, antioxidant 1010 0.2%, UV-292 0.3%, Resorcinol 0.2%, stannous octoate 0.2%, triethylene diamine 0.2%.Component A and component B are mixed, add proper amount of diluting, stir, left standstill 30 minutes, be cast on the glass template under the room temperature and be sprayed on the steel plate, 30 ℃ of following constant temperature 7 days.Coating surface drying time on the glass template is 2 hours, and the coating surface drying time on the steel plate is 1.5 hours; Coating gloss 72.8 on the steel plate, hardness 3H; It is 15.22MPa that filming on the glass template measured its tensile strength according to national polyurethane water-proof paint standard at XLD-3 type electronic tensile test machine, and elongation at break is 365%; The electronic waterproof determinator of LTD-A type is measured its watertightness, and 0.4MPa30min is waterproof.
Embodiment four:
Yellow exposed conveying appliance waterproof paint: concrete proportioning is: component A: 31.95% kilogram of Viscotrol C, 2,4 toluene diisocyanate 9.9%, dimethylbenzene 4.2%, ethyl acetate 2.1%, Diisopropyl azodicarboxylate 0.3%; Component B: glycol ether 10.0%, titanium dioxide 5.2%, medium chrome yellow medium yellow 18.0%, talcum powder 4.2%, toluidine red 0.85%, coupling agent YB-201A (can adopt the titanate coupling agent of Changzhou Ya Bangya space auxiliary agent company limited) 0.5%, vinylbenzene 12.2%, Resorcinol 0.2%, dibutyl tin laurate 0.2%, triethylamine 0.2%.Component A and component B are mixed, add proper amount of diluting, stir, left standstill 30 minutes, be cast on the glass template under the room temperature and be sprayed on the steel plate, 30 ℃ of following constant temperature 7 days.Coating surface drying time on the glass template is 2.5 hours, and the coating surface drying time on the steel plate is 2 hours; Coating gloss 70.9 on the glass template, hardness 4H; It is 7.82 MPa that filming on the glass template measured its tensile strength according to national polyurethane water-proof paint standard at XLD-3 type electronic tensile test machine, and elongation at break is 210%; The electronic waterproof determinator of LTD-A type is measured its watertightness, and 0.4MPa30min is waterproof.
Embodiment five:
Smaragdine(-nus) exposed conveying appliance waterproof paint: concrete proportioning is: component A: Viscotrol C 31.95%, 2,4 toluene diisocyanate 9.9%, dimethylbenzene 4.2%, ethyl acetate 2.1%, Diisopropyl azodicarboxylate 0.3%; Component B: glycol ether 10.0%, titanium dioxide 2.0%, medium chrome yellow medium yellow 3.2%, the titanium cyanines are green 18.85%, talcum powder 4.2%, coupling agent YB-201A (can adopt the titanate coupling agent of Changzhou Ya Bangya space auxiliary agent company limited) 0.5%, vinylformic acid 12.2%, Resorcinol 0.2%, dibutyl tin laurate 0.2%, triethylamine 0.2%.Component A and component B are mixed, add proper amount of diluting, stir, left standstill 30 minutes, be cast on the glass template under the room temperature and be sprayed on the steel plate, 30 ℃ of following constant temperature 7 days.Coating surface drying time on the glass template is 3.5 hours, and the coating surface drying time on the steel plate is 2.5 hours; Coating gloss 67.8 on the glass template, hardness 3H; It is 12.65 MPa that filming on the glass template measured its tensile strength according to national polyurethane water-proof paint standard at XLD-3 type electronic tensile test machine, and elongation at break is 190%; The electronic waterproof determinator of LTD-A type is measured its watertightness, and 0.4MPa30min is waterproof.
Claims (1)
1. the preparation technology of a two-pack Viscotrol C polyurethane water-proof paint is characterized in that, comprises the steps:
(1) raw material is handled: decompression dehydration obtained in 1～2 hour under 100～120 ℃ of blending agentss, the 0.08MPa vacuum tightness; Solid pigment or solid packing are dried under 120 ℃ temperature and were obtained in two hours;
(2) solid pigment that blending agents and toning are needed or solid packing mix with coupling agent and are milled to suitable fineness, and adding vinyl monomer, catalyzer, stopper, photostabilizer stirring more successively, to obtain uniform and stable colored mill base system be B component;
(3) will be dissolved with the organic solvent and 2 of initiator earlier, the 4-tolylene diisocyanate adds the Viscotrol C that in batches adds again in the reactor after the vacuum hydro-extraction, be not more than in water or air cycle condensation and in temperature control under 50 ℃ the condition and reacted 1 ~ 3 hour, stirring and obtaining base polyurethane prepolymer for use as is component A;
(4) component A and B component are mixed by weight 1:0.5 ~ 4, add an amount of organic solvent again and be adjusted to appropriate viscosity, stir, left standstill 10-60 minute, and brushed under the room temperature or be sprayed on to solidify on the different base materials and obtained colored exposed conveying appliance interpenetrating(polymer)networks two-pack Viscotrol C polyurethane water-proof paint in 30 minutes ~ 8 hours;
The used blending agents of described step (1) is 1 ~ 5 kind in glycerine, glycol ether, tetramethylolmethane, sorbyl alcohol, the TriMethylolPropane(TMP); The used solid pigment of step (1) is 1 ~ 10 kind in titanium dioxide, red iron oxide, carbon black, zinc oxide, zinc sulfide white, medium chrome yellow medium yellow, phthalocyanine blue, phthalocyanine green, ultramarine, the toluidine red; Solid packing is that blue or green cream powder, granularity are 1 ~ 5 kind in 600-800 purpose light calcium carbonate, wilkinite, talcum powder, the barite; The used vinyl monomer of step (2) is 1～6 kind in vinylbenzene, methyl methacrylate, butyl methacrylate, vinyl cyanide, the acrylic or methacrylic acid; Coupling agent is titanate coupling agent; Catalyzer is 1～4 kind in dibutyl tin dilaurate, stannous octoate, triethylamine, the triethylene diamine; Stopper is Resorcinol; Photostabilizer is oxidation inhibitor four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, Octabenzone, 2-(2-hydroxyl-3,5-two fourth uncles base phenyl)-5-chlorinated benzotriazole, 2-(2 '-hydroxyl-3 ', 5 '-the diamyl phenyl) in the benzotriazole, UV-292 1～5 kind; The used initiator of step (3) is benzoyl peroxide or Diisopropyl azodicarboxylate; Organic solvent is 1～6 kind in toluene, dimethylbenzene, ethyl acetate, butylacetate, acetone, the methylethylketone;
In component A, by weight percentage, the Viscotrol C consumption is 30% ~ 75%, and the 2,4 toluene diisocyanate consumption is 15% ~ 60%, and consumption of organic solvent is 5% ~ 25%, and initiator amount is 0.2 ~ 2%; In B component, by weight percentage, the blending agents consumption is 10% ~ 30%, solid pigment or solid packing consumption are 20% ~ 45%, and the vinyl monomer consumption is 20 ~ 55%, and the coupling agent consumption is 0.05 ~ 1%, catalyst levels is 0.05 ~ 1%, and the stopper consumption is 0.05 ~ 1%, and the photostabilizer consumption is 0.05 ~ 2%.
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| CN102417790A (en) * | 2011-08-11 | 2012-04-18 | 湖北蓝盾之星科技股份有限公司 | Two-component castor oil polyurethane waterproof paint |
| CN102786873B (en) * | 2012-08-21 | 2015-01-28 | 昆明理工大学 | Nano compound anticorrosive paint and preparation method thereof |
| CN103666235B (en) * | 2013-11-19 | 2018-03-06 | 长安大学 | A kind of polyurethane water-proof anticorrosive paint and preparation method thereof |
| CN105754388A (en) * | 2016-03-02 | 2016-07-13 | 湖北启利新材料股份有限公司 | Double-component nano polyaniline-epoxy acrylic resin/polyurethane interpenetrating-polymer-network conductive anticorrosive coating |
| CN105860817A (en) * | 2016-04-29 | 2016-08-17 | 李强 | Ultravioresistant aqueous polyurethane coating and preparation method thereof |
| WO2018009452A1 (en) * | 2016-07-08 | 2018-01-11 | Basf Se | Hybrid composition |
| CN107365408A (en) * | 2017-09-06 | 2017-11-21 | 厦门厦广安工贸有限公司 | Castor oil based polyurethanes resin and its making |
| CN109735093B (en) * | 2018-12-29 | 2021-01-15 | 扬州市德运塑业科技股份有限公司 | Preparation method of organic silicon/waterborne polyurethane interpenetrating network polymer emulsion containing zinc phthalocyanine for synthetic leather |
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