CN101724326A - Waterborne organic silicon-acrylic acid self-stratifying coating - Google Patents
Waterborne organic silicon-acrylic acid self-stratifying coating Download PDFInfo
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Abstract
The invention relates to a waterborne organic silicon-acrylic acid self-stratifying coating. The invention solves the technical problem of poor self-stratifying property and provides a waterborne organic silicon-acrylic acid self-stratifying coating and a method for preparing the same. In the waterborne organic silicon-acrylic acid self-stratifying coating of the invention, under a condition of lower content of organic silicon, the performance of the conventional silicon acrylic emulsion with high organic silicon content is achieved, and moreover the cost advantage is obvious. The coating is characterized in that: the coating is prepared from the following raw materials in percentage by weight: 10 to 15 percent of organic silicon emulsion, 50 to 60 percent of acrylic emulsion, 5 to 10 percent of organic silicon modified acrylic emulsion, 5 to 7 percent of filling material, 5 to 7 percent of dye, 0.2 to 0.5 percent of thickener, 2 to 3 percent of auxiliary agent, and 10 to 20 percent of water. The preparation method comprises the following steps of: 1, adding the water and auxiliary agent to a paste mixing container; 2, adding fillers and dyes; 3, grinding the mixture to obtain the color paste; 4, adding other raw materials in a paint mixing container; 5, adding the thickener; and 6, filtering the mixed raw materials to obtain the finished product.
Description
Technical field
The present invention relates to a kind of chemistry painting industry, specifically is a kind of waterborne organic silicon-acrylic acid self-stratifying coating.
Background technology
Organosilicon-acrylic coating is the new coating that development in recent years is rapid and have wide market application foreground.It had both had organosilicon fire-resistant, ultra-violet resistance, durability in oxidative degradation, low, the good permeability of surface energy, had snappiness, guarantor's light, tint retention, the high tack of acrylic resin again, was the coating variety of a class excellent combination property.Waterborne organic silicon-acrylic coating environmental friendliness, be widely used as building coating, hide finishes and tackiness agent etc., the exterior coating that particularly can be used for important building or high-rise high-rise building from the nineties in 20th century, becomes the focus product that people competitively develop, produce always.
Waterborne organic silicon-acrylic acid self-stratifying coating has gradient from layer functions.In the coating film process, acrylic resin moves to basic unit, the sticking power of increase and building surface, and the organosilicon component is moved to the top layer, improves the pollution resistance and the weathering resistance of surface coatings.It is ultimate attainment from layering organosilicon-acrylic coating organosilicon performance limited in the coating to be performed to, and can be implemented under the situation of low organosilicon content, reach the performance of the traditional silicon acrylic emulsion of higher organosilicon content, and cost advantage is obvious.
The preparation method of existing waterborne organic silicon-acrylic coating has two kinds: physical blending and chemical modification.For physical blending organosilicon-acrylic coating, be directly to add organic silicon emulsion or dispersion liquid in the acrylic ester emulsion, chemical reaction does not take place between two kinds of emulsions, because organosilicon and vinylformic acid surface energy difference are big, the requirement of each component polymer stable existence in the self stratifying coating is not satisfied in easily layering; Equally for chemical modification organosilicon-acrylic resin, adopt organosilane monomer and Acrylic Acid Monomer emulsion copolymerization, molecule is with chemical bond combination, good stability, in the film-forming process, be difficult to automatic separation, so can not directly be used for preparation from layering organosilicon-acrylic coating.
Employing silicone resins such as Li Yonghua and organosilicon inarch acrylic copolymer and acrylic resin have been feedstock production solvent type organic silicone modified acrylic resin self stratifying coating.These solvents evaporate in construction process in the atmosphere, and not only the health of human body to the constructor works the mischief, and pollutes the environment, and cause the hidden danger of fire in addition.Synthesis technique and organo-siloxane open loop polycondensation and the reaction principle free-radical polymerized with acrylate thereof that Yang Zesheng etc. utilize pre-emulsification to drip have continuously prepared from stratified organosilicon-modified acrylate emulsion.In this method owing to take the method for copolymerization to prepare polymeric constituent in the coating, be difficult to the molecular structure of controlling polymers, cause product from shortcomings such as layering performance poor repeatability.
Summary of the invention
The technical issues that need to address of the present invention are: existing waterborne organic silicon-acrylic coating for reaching coating performance preferably, needs to improve the organosilicon components contents from the layering poor performance.The invention provides a kind of waterborne organic silicon-acrylic acid self-stratifying coating and manufacture method thereof, be implemented under the situation of low organosilicon content, reach the performance of the traditional silicon acrylic emulsion of higher organosilicon content.
For the waterborne organic silicon acrylic coating is had from the layering performance, the technical scheme that adopts physical mixed and chemical modification to combine among the present invention,
Waterborne organic silicon-acrylic acid self-stratifying coating of the present invention is characterized in that: it comprises that the material of following weight percent is a raw material, through preparing product:
Organic silicon emulsion 10～15%,
ACRYLIC EMULSION 50～60%,
Organosilicon-modified acrylic emulsion 5～10%,
Filler 5～7%,
Pigment 5～7%,
Thickening material 0.2～0.5%,
Auxiliary agent 2～3%,
Water 10～20%;
Described organic silicon emulsion is to pass through RSiX
3Monomer and R
1R
2SiX
2Monomer is 1: 10～20 in molar ratio, carries out the emulsion copolymerization reaction and obtains; Wherein: R, R
1, R
2Respectively be selected from a kind of (wherein methyl best results) in methyl, ethyl, propyl group, phenyl, vinyl, trifluoro propyl, aminopropyl, chloropropyl, epoxypropyl, hydroxypropyl, the mercapto propyl group, X is selected from oxyethyl group, methoxyl group;
Described organosilicon-modified acrylic emulsion is by functional group polysiloxane, organosilane monomer, press mass ratio 10～20 with Acrylic Acid Monomer or acrylate monomer: 1: 20～40, get through letex polymerization; Wherein: vinylformic acid or acrylate monomer are the methacrylic acid methyl, Jia Jibingxisuanyizhi, butyl methacrylate, methyl acrylate, ethyl propenoate, butyl acrylate, vinylformic acid, the mixture of one or more in the methacrylic acid, the functional group polysiloxane is ethenyl blocking polydimethylsiloxane or hydroxyl endblocked polydimethylsiloxane, and organosilane monomer is a vinyltrimethoxy silane, vinyltriethoxysilane, methyl ethylene dimethoxy silane, the methyl ethylene diethoxy silane, gamma-methyl allyl acyloxypropyl trimethoxysilane, the gamma-methyl allyl acyloxypropyl triethoxyl silane, the gamma-methyl allyl acyloxypropyl methyl dimethoxysilane, the mixture of one or more in the gamma-methyl allyl acyloxypropyl methyldiethoxysilane;
Its preparation method is following steps:
1) in joining the slurry container, adds entry and auxiliary agent, stir;
2) add filler and pigment in the compound that in step 1), obtains, stir;
3) with step 2) in the mixture that obtains be ground to below the fineness 30 μ m, obtain mill base;
4) in the paint container, add mill base, organic silicon emulsion, organosilicon-modified acrylic emulsion, ACRYLIC EMULSION, stir;
5) add thickening material in the compound that in step 4), obtains, stir;
6) compound that step 5) is obtained filters (filtering larger particles), obtains waterborne organic silicon-acrylic acid self-stratifying coating.
Organic silicon emulsion of the present invention passes through RSiX
3Monomer and R
1R
2SiX
2Monomer adds emulsifying agent and makes through the emulsion copolymerization reaction, contains trifunctional silica chain link (RSiO
1.5), when organic silicon components migrates to coatingsurface, finish the curing of coatingsurface by the polycondensation of functional group, make coatingsurface bright and clean, have best waterproof and dustproof effect.
ACRYLIC EMULSION of the present invention can adopt commercially available ACRYLIC EMULSION, for example B-96 emulsion, AC-261 emulsion.
Organosilicon modified crylic acid resin emulsion of the present invention by functional group polysiloxane, organosilane monomer and Acrylic Acid Monomer or acrylate monomer (letter is vinylformic acid (ester) monomer) add emulsifying agent, initiator gets through letex polymerization.
Because the consistency of silicone resin and acrylic resin is poor, be easy to layering, directly adopt silicone resin and acrylic resin blend, be difficult to stable existence in same system.In system, when adding organosilicon modified crylic acid resin, played the effect of compatilizer, thereby realized the stability of system at both.The applicant discovers, adopt functional group polysiloxane and organosilane monomer jointly and vinylformic acid (ester) class monomer carry out the emulsion copolymerization grafting, the consistency effect that obtains multipolymer is best.Contain two keys in the organosilane monomer, can carry out free-radical polymerizedly, contain alkoxyl group in the organosilane monomer simultaneously,, improve the grafting efficiency of multipolymer with the hydroxyl generation polycondensation in the polysiloxane with vinylformic acid (ester) monomer.When the employing of functional group polysiloxane contained the vinyl polysiloxane, vinyl can carry out free-radical polymerized with organosilane monomer and vinylformic acid (ester) monomer equally.The consumption of organosilicon modified crylic acid resin also has certain scope, and consumption is too big, and the stability of coating strengthens, but in the film forming process of coating, organosilicon and acrylic resin are difficult to layering, have lost from the layering performance.Consumption very little, silicone resin and acrylic resin are difficult to stable existence, have influenced the use properties of coating, cause simultaneously that to be coated with the interlayer bonding force poor, easily come off.The consumption of organosilicon modified crylic acid resin emulsion is 5～10%.
Organic silicon emulsion polymerization of the present invention and organosilicon-modified acrylic emulsion polymeric emulsifying agent are: a kind of in sodium lauryl sulphate, the Sodium dodecylbenzene sulfonate; Used initiator is Potassium Persulphate or ammonium persulphate.
Filler commonly used is a kind of in light calcium carbonate, process white, talcum powder or the mica powder in the production; Pigment is a kind of in iron oxide black, red iron oxide, iron oxide yellow, the titanium dioxide; Thickening material is a kind of in Natvosol, the sodium polyacrylate.
The auxiliary agent that also should add coating weight 2～3% in the preparation process of coating.Auxiliary agent comprises dispersion agent, wetting agent, defoamer, mould inhibitor, sanitas and membrane-forming agent.Used dispersion agent is sodium, ammonium, the amine salt of alkenyl monomer and unsaturated carboxylic acid and lipid multipolymer thereof, and for example: 5040 dispersion agents, 5027 dispersion agents, T-731 dispersion agent, consumption are 0.1～0.3% of coating content; Wetting agent is selected polyether-modified alkynol for use, and as SURFYNOLGA, SURFYNOL TG, consumption is 0.1～0.3% of a coating content; Defoamer is selected organic silicon modified by polyether for use, and as SN313, NXZ, NDW, BYK 024, consumption is 0.01～0.1% of a coating content; Sanitas can be KATHONLXE, HX-89, and consumption is 0.1～0.3% of a coating; Mould inhibitor can be SKANE M-8, BCM sanitas, and consumption is 0.1～0.5% of a coating; Membrane-forming agent is one or more the mixture in ethylene glycol ethyl ether, ethylene glycol monobutyl ether, propylene glycol monomethyl ether, ethylene glycol, the propylene glycol, and consumption is 1.5～2% of a coating content.
The present invention makes the water-soluble organic silicon acrylic coating of development have gradient from layer functions by Molecular Structure Design and component collocation cleverly.In the coating film process, acrylic resin moves to basic unit, the sticking power of increase and building surface, and the organosilicon component is moved to the top layer, improves the pollution resistance and the weathering resistance of surface coatings.Compared with prior art, it is ultimate attainment that organosilicon performance limited in the coating is performed to, and can be implemented under the situation of low organosilicon content, reach the performance of the traditional silicon acrylic emulsion of higher organosilicon content, and cost advantage is obvious.
Embodiment
Below by embodiment, technical scheme of the present invention is described in further detail.
Embodiment 1
The preparation of organic silicon emulsion: in three mouthfuls of reaction flasks of the 500ml that stirring, reflux exchanger and constant pressure funnel are housed, add 100g water, 15g sodium lauryl sulphate, 0.3g sodium hydroxide, start stirring and make emulsifiers dissolve.Be warming up to 80 ℃, drip the mixture of 65g dimethyldiethoxysilane and 5g Union carbide A-162,10min dropwises.Continue reaction 6h.After reaction finishes,, obtain organic silicon emulsion with the Glacial acetic acid neutralization.
The preparation of organosilicon-modified acrylic emulsion: 20g ethenyl blocking polydimethylsiloxane (molecular weight is 2000), 1g vinyltriethoxysilane, 18g butyl acrylate, 18g methyl methacrylate, 0.8g Sodium dodecylbenzene sulfonate and 100g deionized water are joined in the four-necked bottle, fully stir, logical nitrogen 30min deoxygenation, with after the warming-in-water to 70 ℃, add the 0.4g ammonium persulphate, insulation 6h obtains organosilicon-modified acrylic emulsion.
The composition of waterborne organic silicon-acrylic acid self-stratifying coating: organic silicon emulsion 10g, ACRYLIC EMULSION 57g, organosilicon-modified acrylic emulsion 8g, light calcium carbonate 6g, titanium dioxide 6g, Natvosol 0.3g, 5040 dispersion agent 0.1g, SURFYNOL GA 0.2g, SN 313 0.05g, KATHON LXE 0.2g, SKANE M-8 0.5g, ethylene glycol 1.5g, water 10.15g.
Waterborne organic silicon-acrylic acid self-stratifying coating prepares by following steps:
1) in joining the slurry container, adds 10.15g water and 0.1g 5040 dispersion agents, 0.2g SURFYNOL GA, 0.05g SN313,0.2g KATHON LXE, 0.5g SKANE M-8,1.5g ethylene glycol, stir;
2) add 6g light calcium carbonate and 6g titanium dioxide in the compound that in step 1), obtains, stir;
3) with step 2) in the mixture that obtains be ground to fineness 25 μ m, obtain mill base;
4) in the paint container, add mill base, 10g organic silicon emulsion, 8g organosilicon-modified acrylic emulsion, 57g AC-261 Emulsion acrylic resin, stir;
5) add the 0.3g Natvosol in the compound that in step 4), obtains, stir;
6) compound that step 5) is obtained filters, and the filtering larger particles obtains waterborne organic silicon-acrylic acid self-stratifying coating.
Prepared organosilicon-acrylic coating is cured, and with each layer silicone content in the X-gamma spectrometer test latex film cross section, the result is:
| The latex film cross section number of plies | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 |
| Silicon content (%) | 3.5 | 3.6 | 3.2 | 3.0 | 2.6 | 2.1 | 1.7 | 1.5 | 1.3 | 1.2 |
Annotate: the latex film cross section is divided into 10 layers, and the 1st layer is upper surface, and 10 layers is lower surface.
As can be seen, the content difference of different sectional position element silicons illustrates that the coating of preparation has significantly from layer functions.
Embodiment 2
The preparation of organic silicon emulsion: in three mouthfuls of reaction flasks of the 500ml that stirring, reflux exchanger and constant pressure funnel are housed, add 100g water, 10g Sodium dodecylbenzene sulfonate, 0.5g sodium hydroxide, start stirring and make emulsifiers dissolve.Be warming up to 70 ℃, drip the mixture of 60g dimethyldimethoxysil,ne and 9.0g aminopropyl trimethoxysilane, 15min dropwises.Continue reaction 6h.After reaction finishes,, obtain organic silicon emulsion with the Glacial acetic acid neutralization.
The preparation of organosilicon-modified acrylic emulsion: 20g hydroxyl endblocked polydimethylsiloxane (molecular weight is 3500), 1g gamma-methyl allyl acyloxypropyl trimethoxysilane, 1g methyl ethylene diethoxy silane, 20g butyl acrylate, 25g vinylformic acid, 1.2g sodium lauryl sulphate and 150g deionized water are joined in the four-necked bottle, fully stir, logical nitrogen 30min deoxygenation, with after the warming-in-water to 70 ℃, add the 0.6g Potassium Persulphate, insulation 6h obtains organosilicon-modified acrylic emulsion.
The composition of waterborne organic silicon vinylformic acid self stratifying coating: organic silicon emulsion 15g, ACRYLIC EMULSION 50g, organosilicon-modified acrylic emulsion 5g, talcum powder 5g, red iron oxide 5g, sodium polyacrylate 0.3g, 5027 dispersion agent 0.3g, SURFYNOL TG 0.1g, NDW 0.1g, HX-89 0.1g, BCM sanitas 0.1g, propylene glycol monomethyl ether 2.0g, water 17g.
Waterborne organic silicon-acrylic acid self-stratifying coating prepares by following steps:
1) in joining the slurry container, adds 17g water and 0.3g 5027 dispersion agents, 0.1g SURFYNOL TG, 0.1g NDW, 0.1gKHX-89,0.1g BCM sanitas, 2.0g propylene glycol monomethyl ether, stir;
2) add 5g talcum powder and 5g red iron oxide in the compound that in step 1), obtains, stir;
3) with step 2) in the mixture that obtains be ground to fineness 28 Jing, obtain mill base;
4) in the paint container, add mill base, 15g organic silicon emulsion, 5g organosilicon-modified acrylic emulsion, 50g B-96 ACRYLIC EMULSION, stir;
5) add the 0.3g sodium polyacrylate in the compound that in step 4), obtains, stir;
6) compound that step 5) is obtained filters, and the filtering larger particles obtains waterborne organic silicon-acrylic acid self-stratifying coating.
Prepared organosilicon-acrylic coating is cured, and with each layer silicone content in the X-gamma spectrometer test latex film cross section, the result is:
| The latex film cross section number of plies | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 |
| Silicon content (%) | 4.7 | 4.5 | 4.4 | 4.2 | 3.5 | 3.1 | 2.5 | 1.9 | 1.4 | 1.2 |
Annotate: the latex film cross section is divided into 10 layers, and the 1st layer is upper surface, and 10 layers is lower surface.
As can be seen, the content difference of different sectional position element silicons illustrates that the coating of preparation has significantly from layer functions.
Embodiment 3
The preparation of organic silicon emulsion: in three mouthfuls of reaction flasks of the 500ml that stirring, reflux exchanger and constant pressure funnel are housed, add 100g water, 10g Sodium dodecylbenzene sulfonate, 0.5g sodium hydroxide, start stirring and make emulsifiers dissolve.Be warming up to 80 ℃, drip the mixture of 75g aminomethyl phenyl dimethoxy silane and 4.1g mercaptopropyl trimethoxysilane, 20min dropwises.Continue reaction 6h.After reaction finishes,, obtain organic silicon emulsion with the Glacial acetic acid neutralization.
The preparation of organosilicon-modified acrylic emulsion: 15g hydroxyl endblocked polydimethylsiloxane (molecular weight is 2800), 1g gamma-methyl allyl acyloxypropyl triethoxyl silane, 10g methacrylic acid, 20g methyl acrylate, 0.8g Sodium dodecylbenzene sulfonate and 120g deionized water are joined in the four-necked bottle, fully stir, logical nitrogen 30min deoxygenation, with after the warming-in-water to 80 ℃, add the 0.5g ammonium persulphate, insulation 6h obtains organosilicon-modified acrylic emulsion.
The composition of waterborne organic silicon vinylformic acid self stratifying coating: organic silicon emulsion 12g, ACRYLIC EMULSION 50g, organosilicon-modified acrylic emulsion 7g, mica powder 6g, iron oxide yellow 5g, sodium polyacrylate 0.5g, T-731 dispersion agent 0.1g, SURFYNOL TG 0.1g, NXZ 0.05g, HX-89 0.1g, BCM sanitas 0.1g, ethylene glycol 0.8g, ethylene glycol ethyl ether 1.5g, water 11.75g.
The manufacture method of waterborne organic silicon vinylformic acid self stratifying coating may further comprise the steps:
1) in joining the slurry container, adds 11.75g water and 0.1g T-731 dispersion agent, 0.1g SURFYNOL TG, 0.05g NXZ, 0.1g KHX-89,0.1g BCM sanitas, 0.8g ethylene glycol, 1.5g ethylene glycol ethyl ether, stir;
2) add 6g mica powder and 5g iron oxide yellow in the compound that in step (1), obtains, stir;
3) mixture that obtains in the step (2) is ground to fineness 29 μ m, obtains mill base;
4) in the paint container, add mill base, 12g organic silicon emulsion, 7g organosilicon-modified acrylic emulsion, 50gB-96 ACRYLIC EMULSION, stir;
5) add the 0.5g sodium polyacrylate in the compound that in step (4), obtains, stir;
6) compound that step (5) is obtained filters, and the filtering larger particles obtains waterborne organic silicon-acrylic acid self-stratifying coating.
Prepared organosilicon-acrylic coating is cured, and with each layer silicone content in the X-gamma spectrometer test latex film cross section, the result is:
| The latex film cross section number of plies | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 |
| Silicon content (%) | 4.2 | 4.1 | 3.9 | 3.5 | 3.1 | 2.9 | 1.9 | 1.6 | 1.4 | 1.2 |
Annotate: latex film is divided into 10 layers, and the 1st layer is upper surface, and 10 layers is lower surface.
As can be seen, the content difference of different sectional position element silicons illustrates that the coating of preparation has significantly from layer functions.
Claims (2)
1. waterborne organic silicon vinylformic acid self stratifying coating, it is characterized in that: the material of its following column weight amount per-cent is a raw material, through preparing product:
Organic silicon emulsion 10～15%,
ACRYLIC EMULSION 50～60%,
Organosilicon-modified acrylic emulsion 5～10%,
Filler 5～7%,
Pigment 5～7%,
Thickening material 0.2～0.5%,
Auxiliary agent 2～3%,
Water 10～20%;
Described organic silicon emulsion system is 1: 10～20 by RSiX3 and R1R2SiX2 in molar ratio, carries out emulsion copolymerization and reacts and obtain; Wherein: R, R1, R2 respectively are selected from a kind of in methyl, ethyl, propyl group, phenyl, vinyl, trifluoro propyl, aminopropyl, chloropropyl, epoxypropyl, hydroxypropyl, the mercapto propyl group, and X is selected from oxyethyl group, methoxyl group;
Described organosilicon-modified acrylic emulsion is by functional group polysiloxane, organosilane monomer, press mass ratio 10～20 with Acrylic Acid Monomer or acrylate monomer: 1: 20～40, get through letex polymerization; Wherein: vinylformic acid or acrylate monomer are the methacrylic acid methyl, Jia Jibingxisuanyizhi, butyl methacrylate, methyl acrylate, ethyl propenoate, butyl acrylate, vinylformic acid, the mixture of one or more in the methacrylic acid, the functional group polysiloxane is ethenyl blocking polydimethylsiloxane or hydroxyl endblocked polydimethylsiloxane, and organosilane monomer is a vinyltrimethoxy silane, vinyltriethoxysilane, methyl ethylene dimethoxy silane, the methyl ethylene diethoxy silane, gamma-methyl allyl acyloxypropyl trimethoxysilane, the gamma-methyl allyl acyloxypropyl triethoxyl silane, the gamma-methyl allyl acyloxypropyl methyl dimethoxysilane, the mixture of one or more in the gamma-methyl allyl acyloxypropyl methyldiethoxysilane;
Its preparation method is following steps:
1) in joining the slurry container, adds entry and auxiliary agent, stir;
2) add filler and pigment in the compound that in step 1), obtains, stir;
3) with step 2) in the mixture that obtains be ground to below fineness 30 Jing, obtain mill base;
4) in the paint container, add mill base, organic silicon emulsion, organosilicon-modified acrylic emulsion, ACRYLIC EMULSION, stir;
5) add thickening material in the compound that in step 4), obtains, stir;
6) compound that step 5) is obtained filters, and obtains waterborne organic silicon vinylformic acid self stratifying coating.
2. waterborne organic silicon vinylformic acid self stratifying coating according to claim 1 is characterized in that:
Described filler is a kind of in light calcium carbonate, process white, talcum powder or the mica powder;
Described pigment is a kind of in iron oxide black, red iron oxide, iron oxide yellow, the titanium dioxide;
Described thickening material is a kind of in Natvosol, the sodium polyacrylate;
Described auxiliary dosage is a coating weight 2～3%, wherein dispersion agent be coating weight 0.1～0.3%, wetting agent be coating weight 0.1～0.3%, defoamer be coating weight 0.01～0.1%, mould inhibitor be coating weight 0.1～0.5%, sanitas is that 0.1～0.3% and membrane-forming agent of coating weight is 1.5～2% of coating weight.
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