CN102093761A - Preparation method of aqueous aluminum silver paste - Google Patents
Preparation method of aqueous aluminum silver paste Download PDFInfo
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- CN102093761A CN102093761A CN2010105355187A CN201010535518A CN102093761A CN 102093761 A CN102093761 A CN 102093761A CN 2010105355187 A CN2010105355187 A CN 2010105355187A CN 201010535518 A CN201010535518 A CN 201010535518A CN 102093761 A CN102093761 A CN 102093761A
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Abstract
The invention provides a preparation method of aqueous aluminum silver paste. The preparation method comprises the following steps of: 1, adding an aluminum powder pigment and acetone into a vessel, stirring and filtering to obtain washed aluminum powder; 2, adding the washed aluminum powder obtained in the step 1 into an alcohol solvent, ultrasonically dispersing, adding into a reaction vessel, adding organic silicon, stepwise adding ammonia water, abnd stirring to make the mixture react 3, filtering the product obtained in the step 2 and drying in a vacuum drying box; 4, adding the product obtained in the step 3 into an acetone solution of a comb-like polymer comprising an anchor group and a hydrophilic group and stirring; and 5, removing the acetone from the product obtained in the step 4 by decompressing and distilling to obtain the aqueous aluminum silver paste. According to the preparation method of the aqueous aluminum silver paste, coating completeness is enhanced, falling, dusting and agglomeration of a coating are prevented, and the coating has high dispersity, so that the using performance of the prepared aqueous aluminum silver paste is integrally enhanced.
Description
Technical field
The present invention relates to a kind of preparation method of water-based metal pigment, especially relate to a kind of preparation method of water aluminum-silver slurry.
Background technology
Aluminium powder pigment has excellent glossiness and tone, is one of important metallic pigment.Along with development of science and technology, the kind of aluminium powder pigment is more and more, now has been widely used in the multiple industry and the commercial fields such as internal and external ornament of automobile, motorcycle, sports equipment, electric equipment products, buildings.
Along with the pay attention to day by day of people to environment protection, the aluminium powder that can be applied to water-based system is that water aluminum-silver slurry has also obtained a large amount of research.Water aluminum-silver slurry has unique environmental friendliness function, can be widely used in water-borne coatings and water color ink.Water aluminum-silver slurry can not only make film forming matter have advantages such as acidproof, alkaline-resisting, high temperature resistant, and can compare favourably with the oiliness aluminium-silver slurry at aspects such as metalluster, opacifying powers.
But, because aluminium is easy to and water reacts, when being applied to water-based system, this reaction not only can destroy the metalluster of aluminium powder, and consequent hydrogen (promptly " getting angry "), cause burning or blast easily, therefore to produce the reaction that water aluminum-silver slurry at first will stop aluminium powder and water.What adopt at present is two kinds of technology based on different principle: the one, and additive technology, promptly on the aluminium powder pigment particle surface with the physical method mixed additive, form a protective layer by modes such as electrostatic adhesion at the aluminium flake skin, protective layer plays iris action, stop the reaction of aluminium and water, but the protective layer instability that forms, disassociation easily in medium; The 2nd, coating technology, one aluminium powder particle is wrapped, thereby stops the reaction of aluminium and water, and this coating is stable, can form powerful combinations such as hydrogen bond, is not easy to break away from medium.
Coating technology normally contains chromium cpd or silicon dioxide film at aluminium powder surface coverage one deck.Chromium ion pollutes the environment, and its application is restricted.Silicon dioxide film has excellent inertia and wetting ability, lower film-forming temperature, and the transparency of its uniqueness can not damaged the luster performance of aluminium powder, thereby is more studied.Present research concentrates on adopts sol-gel method to form silicon dioxide film, promptly utilizes organosilyl hydrolysis-condensation to coat the uniform SiO of last layer on the surface of flake aluminum
2Film.
But in the prior art, because the speed of sol-gel is difficult to homogeneous, and the irregularity of aluminium powder micro-shape, the silicon dioxide film that makes sol-gel method form exists and coats imperfect, problem such as come off easily, thereby can not stop the generation of hydrogen fully.
Simultaneously, there is a large amount of hydroxyls in the silicon dioxide film surface, and hydroxyl makes coating aluminium powder surface present wetting ability, the formation tridimensional network but this surface absorbs water again easily.The intermolecular reactive force of this tridimensional network is very strong, make and attract each other, tangle between the aluminium powder particle, thereby the aluminium powder particulate of coated with silica is agglomerated into aggregate easily, is unfavorable for the dispersion in application system, is unfavorable for embodying the advantage of water aluminum-silver slurry.
In addition, traditional oiliness aluminium powder has grinding aid in surface bonding in kneading process, as oil soluble long-chain materials such as stearic acid, oleic acid, grinding aid can not only effectively alleviate the deadweight of aluminium powder, and it is floating in medium to be convenient to aluminium powder, and can improve the consistency of aluminium powder and resin.But for making the water-based aluminium powder possess the good hydrophilicity energy, can not be at oil-soluble substances such as aluminium powder surface bonding stearic acid, oleic acid, this makes the consistency and the showy degradation of aluminium powder in medium of water-based aluminium powder and resin.The coated with silica aluminium powder also can reduce surface tension in addition, thereby makes consistency descend more, can cause the problem of after the film forming drying " dry linting ".The showy degradation of water-based aluminium powder can make aluminium powder precipitate gathering in water-based system, is unfavorable for using.
For example, provided a kind of preparation method of silicon dioxide coating type water aluminum-silver slurry in disclosed Chinese patent application announcement on August 6th, 2008 CN101235226A, this preparation method coats aluminium powder by silicon dioxide film, obtain in the aqueous solution, to have good dispersion, and water aluminum-silver slurry with excellent acid-fast alkali-proof performance, but this method belongs to individual layer to coat, and exists coating layer to come off, coat defectives such as imperfect and dry linting easily, can't stop the generation of hydrogen fully.
For example, the Chinese patent CN100465235C of Granted publication provided a kind of preparation method of coated aluminium powder pigment on March 4th, 2009, this method is utilized organo-siloxane to form the first layer on the aluminium powder pigment surface and is coated, utilize reacting generating copolymer that aluminium powder is carried out coating the second time, preferably resolve traditional aluminium powder " getting angry " problem in use and storage process, kept good metal gloss simultaneously, but this method is to carry out polyreaction in the coating system, can destroy original silicon dioxide film that forms, and the polymer coated silica film that reaction obtains, when realizing complete coating, also destroyed the wetting ability of silicon dioxide film, add that polymkeric substance self lacks hydrophilic segment, thereby this system wetting ability deficiency, will cause coating the difficulties in dispersion of aluminium powder in water-based system.
This shows, prior art solutions all can not coat complete, coating layer does not come off, solved in no dry linting, dispersiveness and the reunion comprehensively.
Summary of the invention
At the deficiencies in the prior art, the preparation method who the purpose of this invention is to provide a kind of water aluminum-silver slurry, the water aluminum-silver slurry that described preparation method makes can coat complete, coating does not come off, no dry linting, stably dispersing and do not have in the reunion solution prior art problems comprehensively.
For achieving the above object, the invention provides a kind of preparation method of water aluminum-silver slurry, comprise step: step 1: in container, add aluminium powder pigment and acetone, stirred 0.5~1 hour, filter and obtain washed aluminium powder; Step 2: get in the alcoholic solvent that 1~10 part of washed aluminium powder in the step 1 joins 80~100 parts, behind ultra-sonic dispersion, join in the reaction vessel, add 0.2~3 part of organosilicon, progressively add 4~18 parts of ammoniacal liquor again, stir reaction down 2~10 hours, temperature of reaction is 40~50 ℃; Step 3: after the product that step 2 is obtained filters, carry out drying in 80~100 ℃ in vacuum drying oven, be 1~2 hour time of drying; Step 4: get in the acetone soln that 1~10 part of the product that obtains in the step 3 joins the comb-shaped polymer that contains 0.1~2 part, stirred 0.5~2 hour, comb-shaped polymer is 40~80 with the ratio of acetone, and wherein, described comb-shaped polymer comprises anchoring group and hydrophilic radical; Step 5: the product that step 4 obtains is removed acetone by underpressure distillation, and temperature is no more than 50 ℃, obtains solid content and be 90~95% water aluminum-silver slurry.
Compared with prior art, preparation method according to water aluminum-silver slurry of the present invention has following beneficial effect: by adopting acetone aluminium powder is cleaned washing, aluminium powder surface coverage silicon dioxide film, the aluminium powder after coating is carried out the vacuum drying drying and adopt the comb-shaped polymer with anchoring group and hydrophilic group to carry out secondary coating, thereby improved the integrity that coats, coating do not have come off, no dry linting, dispersed good and do not have agglomeration and take place, thereby improve the use properties of prepared water aluminum-silver slurry on the whole.
Embodiment
Describe preparation method and embodiment now in detail according to water aluminum-silver slurry of the present invention.
At first, simple declaration is once according to the preparation method's of water aluminum-silver slurry of the present invention technical conceive.
The preparation method's of foundation water aluminum-silver slurry of the present invention technical conceive is: at first be to coat layer of silicon dioxide film (the first layer coating) on the surface of flake aluminum particle, make the aluminium powder surface become wetting ability by hydrophobicity, stop aluminium powder and water to react simultaneously; Secondly, the synthetic comb shaped polymer that is applicable to water-based system, this comb shaped polymer has on one side that the anchoring base can tightly be adsorbed on silicon dioxide film and the surface of the aluminium powder that do not coat fully, the formation second layer coats, further stop aluminium powder and water to react, and the other side of this comb-shaped polymer have hydrophilic group, can be so that aluminium powder obtains stable dispersion in water-based system, and improve the consistency of aluminium powder and resin, solve " dry linting " problem.
Secondly, describe the preparation method of foundation water aluminum-silver slurry of the present invention in detail.
Preparation method according to water aluminum-silver slurry of the present invention comprises step:
Step 1: in container, add aluminium powder pigment and acetone, stirred 0.5~1 hour, filter and obtain washed aluminium powder;
Step 2: get in the alcoholic solvent that 1~10 part of washed aluminium powder in the step 1 joins 80~100 parts, behind ultra-sonic dispersion, join in the reaction vessel, add 0.2~3 part of organosilicon, progressively add 4~18 parts of ammoniacal liquor again, stir reaction down 2~10 hours, temperature of reaction is 40~50 ℃;
Step 3: after the product that step 2 is obtained filters, carry out drying in 80~100 ℃ in vacuum drying oven, be 1~2 hour time of drying;
Step 4: get in the acetone soln that 1~10 part of the product that obtains in the step 3 joins the comb-shaped polymer that contains 0.1~2 part, stirred 0.5~2 hour, comb-shaped polymer is 40~80 with the ratio of acetone, and wherein, described comb-shaped polymer comprises anchoring group and hydrophilic group;
Step 5: the product that step 4 obtains is removed acetone by underpressure distillation, and temperature is no more than 50 ℃, obtains solid content and be 90~95% water aluminum-silver slurry.
The turnout of oiliness aluminium powder is bigger at present, directly adopt the modification of oiliness aluminium powder, can avoid grinding link, help reducing cost, but the oiliness aluminium powder has added grinding aids such as stearic acid or petroleum hydrocarbon in the process of grinding, coated one deck organic membrane on its surface, make the aluminium powder surface have very strong hydrophobicity, dispersed extreme difference in water-based system.Therefore, according among the preparation method of water aluminum-silver slurry of the present invention, in step 1, adopt acetone that aluminium powder is carried out carrying out washing treatment, effectively the flush away organic membrane is convenient to coating modification.
According among the preparation method of water aluminum-silver slurry of the present invention, in step 2, described alcoholic solvent can be the group that n-propyl alcohol, Virahol or their mixture are formed.Pass through step 2, coat one deck inert silicon dioxide film on washed aluminium powder surface, make the aluminium powder surface become wetting ability by hydrophobicity, stop the aluminium powder surface to react simultaneously with water, effectively solve the problem of getting angry of aluminium powder, improve the period of storage of water aluminum-silver slurry, because silicon dioxide film belongs to transparency material, do not influence the metalluster of aluminium powder simultaneously.
In the foundation preparation method of water aluminum-silver slurry of the present invention, in step 2, described organosilicon is tetraethoxy or methyl silicate.
In the foundation preparation method of water aluminum-silver slurry of the present invention, in step 3, organosilicon is by hydrolysis generation polycondensation, but this reaction is based on linear condensation, form silicon dioxide film in conjunction with not fine and close, come off easily,, make silicon dioxide film form network structure so the present invention carries out the vacuum drying drying to the aluminium powder after coating, in conjunction with tight, intensity combination big and aluminium powder is more firm, difficult drop-off.
In the foundation preparation method of water aluminum-silver slurry of the present invention, in step 4, the structural formula of described comb-shaped polymer is:
In the foundation preparation method of water aluminum-silver slurry of the present invention, the preparation process of described comb-shaped polymer is as follows:
The first step: in reaction vessel, add quantitative poly glycol monomethyl ether, be warming up to 100~120 ℃, vacuumize the moisture that 0.1~2h removes poly glycol monomethyl ether absorption.
Second step: under nitrogen protection, adding solvent and maleic anhydride (maleic anhydride: poly glycol monomethyl ether=1~1.5: 1, mol ratio), reaction 1~2h obtains macromonomer poly glycol monomethyl ether toxilic acid esterification thing.
The 3rd step: add the initiator Diisopropyl azodicarboxylate, elevated temperature to 70~75 ℃, splash into methyl acrylate (methyl acrylate: maleic anhydride=1~2: 1, mol ratio), isothermal reaction 2h, reaction is used sherwood oil and deionized water wash resultant respectively after finishing, in vacuum drying oven, be dried to constant weight, promptly obtain comb-shaped polymer.
According among the preparation method of water aluminum-silver slurry of the present invention, the number-average molecular weight of described comb-shaped polymer is 10000~70000, tightly is adsorbed on the silicon dioxide film and the surface of the aluminium powder of coating fully not to guarantee comb-shaped polymer.
In the foundation preparation method of water aluminum-silver slurry of the present invention, the number-average molecular weight of described poly glycol monomethyl ether is 400~2000.
In the foundation preparation method of water aluminum-silver slurry of the present invention, the synthetic comb-shaped polymer possesses anchoring group COOH, COOH can pass through hydrogen bonded, tightly is adsorbed on silicon dioxide film and the surface of the aluminium powder that do not coat fully, stops the generation of getting angry and the reunion of aluminium powder; The hydrophilic group of synthetic comb-shaped polymer is a poly glycol monomethyl ether, and hydrophilic group and glassware for drinking water have good consistency, can form the suitable protective layer of thickness at the aluminium powder microparticle surfaces.This protective layer can make when the aluminium powder particulate is close mutually, flicks owing to the interaction between the protective layer makes particulate, thereby realizes the stable dispersion of aluminium powder in water-based system, greatly reduces and reunites; In addition, the poly glycol monomethyl ether long-chain can improve the consistency that coats aluminium powder and filmogen, " dry linting " problem after the reduction film forming.
At last, provide the preparation method's of several water aluminum-silver slurries of the present invention embodiment, but these embodiment do not limit the scope of the invention.
Embodiment 1
1, in container, adds 1 part of aluminium powder pigment and 100 parts of acetone, stir 0.5h, filter and obtain washed aluminium powder; 2, get in the n-propyl alcohol that washed aluminium powder joins 80 parts, behind ultra-sonic dispersion, join in the reaction vessel, add 0.2 part of tetraethoxy and progressively add 4 parts of ammoniacal liquor again, stir reaction 10h down, temperature of reaction is 40 ℃; 3, aluminium powder is filtered after, in vacuum drying oven, carry out drying in 80 ℃, be 2h time of drying, obtains the aluminium powder that silicon dioxide film coats; 4, join again in 40 parts of acetone solns of the comb-shaped polymer that contains 0.1 part, stir 0.5h; 5, underpressure distillation boils off most of acetone, and temperature is no more than 50 ℃, promptly obtains solid content and be 90% water aluminum-silver slurry.
Wherein, the preparation of comb-shaped polymer is: after 1 part of poly glycol monomethyl ether (Mn=800) drying, under nitrogen protection; the maleic anhydride that adds 20 parts of hexanaphthenes and 1 part; reaction 1h adds 0.1 part of Diisopropyl azodicarboxylate, elevated temperature to 70 ℃; splash into 1 part of methyl acrylate; isothermal reaction 2h, reaction is respectively washed three times with sherwood oil and deionized water respectively after finishing; in vacuum drying oven, be dried to constant weight, promptly obtain comb-shaped polymer (Mn=10000).
Embodiment 2
1, in container, adds 10 parts of aluminium powder pigments and 100 parts of acetone, stir 1h, filter and obtain washed aluminium powder; 2, get in the Virahol that washed aluminium powder joins 100 parts, behind ultra-sonic dispersion, join in the reaction vessel, add 3 parts of methyl silicates, progressively add 18 parts of ammoniacal liquor again, stir reaction 2h down, temperature of reaction is 50 ℃; 3, aluminium powder is filtered after, in vacuum drying oven, carry out drying in 100 ℃, be 1h time of drying, obtains the aluminium powder that silicon dioxide film coats; 4, join again in 80 parts of acetone solns of the comb-shaped polymer that contains 2 parts, stir 2h; 5, underpressure distillation boils off most of acetone, and temperature is no more than 50 ℃, promptly obtains solid content and be 95% water aluminum-silver slurry.
Wherein the preparation of comb-shaped polymer is: after 1 part of poly glycol monomethyl ether (Mn=2000) drying; under nitrogen protection, add the maleic anhydride of 20 parts of hexanaphthenes and 1.5 parts, reaction 2h; add 0.1 part of Diisopropyl azodicarboxylate; elevated temperature to 70 ℃ splashes into 2 parts of methyl acrylates, isothermal reaction 2h; after reaction finishes; respectively wash three times with sherwood oil and deionized water respectively, in vacuum drying oven, be dried to constant weight, promptly obtain comb-shaped polymer (Mn=70000).
Embodiment 3
1, in container, adds 6 parts of aluminium powder pigments and 100 parts of acetone, stir 0.5h, filter and obtain washed aluminium powder; 2, get in the Virahol that washed aluminium powder joins 90 parts, behind ultra-sonic dispersion, join in the reaction vessel, add 0.3 part of tetraethoxy and progressively add 10 parts of ammoniacal liquor again, stir reaction 3h down, temperature of reaction is 45 ℃; 3, aluminium powder is filtered after, in vacuum drying oven, carry out drying in 90 ℃, be 2h time of drying, obtains the aluminium powder that silicon dioxide film coats.4, join again in 50 parts of acetone solns of the comb-shaped polymer that contains 0.5 part, stir 1h; 5, underpressure distillation boils off most of acetone, and temperature is no more than 50 ℃, promptly obtains solid content and be 92% water aluminum-silver slurry.
Wherein the preparation of comb-shaped polymer is: after 2 parts of poly glycol monomethyl ethers (Mn=400) and 1 part of poly glycol monomethyl ether (Mn=1200) drying; under nitrogen protection; the maleic anhydride that adds 30 parts of hexanaphthenes and 4 parts; reaction 1h; add 0.4 part of Diisopropyl azodicarboxylate; elevated temperature to 75 ℃; splash into 8 parts of methyl acrylates; isothermal reaction 2h; after reaction finishes; respectively wash three times with sherwood oil and deionized water respectively, in vacuum drying oven, be dried to constant weight, promptly obtain comb-shaped polymer (Mn=46000).
Embodiment 4
Dispose the solution of pH=5 respectively with sodium hydroxide configuration pH=10 and hydrochloric acid, coating aluminium powder with embodiment 1, embodiment 2 and embodiment 3 preparations adds respectively in two kinds of solution again, at room temperature, the aluminium powder that is used in the Chinese patent CN201429441Y design of Granted publication on March 24th, 2010 determinator of getting angry is measured the performance of getting angry that coats aluminium powder.The results are shown in Table one:
Table one Performance Detection of getting angry
The coating aluminium powder of the present invention's preparation coats complete, has the superior acid resistance energy, preferably alkaline resistance properties.
Embodiment 5
The coating aluminium powder of embodiment 1, embodiment 2 and embodiment 3 preparations is carried out the glossiness contrast with the aluminium powder that does not coat, the result shows, the glossiness that coats aluminium powder is not for coating 85~95% of aluminium powder glossiness, and the preparation method that the present invention adopts has kept the glossiness of aluminium powder preferably.
Embodiment 6
The coating aluminium powder of getting 5 gram embodiment 1, embodiment 2 and embodiment 3 preparations joins respectively in the 100 gram water, shakes, and as seen coats aluminium powder and all disperses rapidly, the visible aggregate of reuniting of no naked eyes.Distinguish the size-grade distribution of the coating aluminium powder of test implementation example 1, embodiment 2 and embodiment 3 preparations again with laser particle analyzer, the result shows that the size-grade distribution trend and the raw material aluminium powder that coat back aluminium powder particle are more or less the same, and median size slightly increases.The preparation method that the present invention adopts has realized the dispersion of aluminium powder preferably.
Embodiment 7
The coating aluminium powder and the water-base resin of commercially available water-based aluminium powder and embodiment 1, embodiment 2 and embodiment 3 preparations are mixed into coating, and dry back closely sticks on coatingsurface with special adhesive tape, tears fast then, observes the dry linting situation of coatingsurface aluminium powder.The result shows that the dry linting of filming of commercially available water-based aluminium powder preparation is serious, the not dry linting of filming all that the coating aluminium powder of embodiment 1, embodiment 2 and embodiment 3 preparations forms.The solution that the preparation method that the present invention adopts keeps preferably the dry linting problem of aluminium powder.
From the foregoing description as can be seen, adopt the water aluminum-silver slurry of the preparation method preparation of water aluminum-silver slurry of the present invention not come off in covering property integrity, coating, no dry linting, dispersiveness and reunite on comprehensive solution prior art problems, and safety and stability, be applicable to water-based system, be convenient to use in industries such as water-borne coatings, water color inks.
Claims (7)
1. the preparation method of a water aluminum-silver slurry comprises step:
Step 1: in container, add aluminium powder pigment and acetone, stirred 0.5~1 hour, filter and obtain washed aluminium powder;
Step 2: get in the alcoholic solvent that 1~10 part of washed aluminium powder in the step 1 joins 80~100 parts, behind ultra-sonic dispersion, join in the reaction vessel, add 0.2~3 part of organosilicon, progressively add 4~18 parts of ammoniacal liquor again, stir reaction down 2~10 hours, temperature of reaction is 40~50 ℃;
Step 3: after the product that step 2 is obtained filters, carry out drying in 80~100 ℃ in vacuum drying oven, be 1~2 hour time of drying;
Step 4: get in the acetone soln that 1~10 part of the product that obtains in the step 3 joins the comb-shaped polymer that contains 0.1~2 part, stirred 0.5~2 hour, comb-shaped polymer is 40~80 with the ratio of acetone, and wherein, described comb-shaped polymer comprises anchoring group and hydrophilic group; And
Step 5: the product that step 4 obtains is removed acetone by underpressure distillation, and temperature is no more than 50 ℃, obtains solid content and be 90~95% water aluminum-silver slurry.
2. the preparation method of water aluminum-silver slurry according to claim 1 is characterized in that, described alcoholic solvent is the group that n-propyl alcohol, Virahol or their mixture are formed.
3. the preparation method of water aluminum-silver slurry according to claim 1 is characterized in that, described organosilicon is tetraethoxy or methyl silicate.
5. according to the preparation method of the water aluminum-silver slurry of claim 4, it is characterized in that the preparation process of described comb-shaped polymer is as follows:
The first step: in reaction vessel, add quantitative poly glycol monomethyl ether, be warming up to 100~120 ℃, vacuumize the moisture that 0.1~2h removes poly glycol monomethyl ether absorption;
Second step: under nitrogen protection, add solvent and maleic anhydride, wherein maleic anhydride and poly glycol monomethyl ether are 1~1.5: 1 mol ratio, and reaction 1~2h obtains macromonomer poly glycol monomethyl ether toxilic acid esterification thing;
The 3rd step: add the initiator Diisopropyl azodicarboxylate, elevated temperature to 70~75 ℃, splash into methyl acrylate, wherein methyl acrylate and maleic anhydride are 1~2: 1 mol ratio, isothermal reaction 2h, reaction is used sherwood oil and deionized water wash resultant respectively after finishing, in vacuum drying oven, be dried to constant weight, promptly obtain comb-shaped polymer.
6. comb-shaped polymer according to claim 4 is characterized in that, the number-average molecular weight of described comb-shaped polymer is 10000~70000.
7. comb-shaped polymer according to claim 4 is characterized in that, the number-average molecular weight of described poly glycol monomethyl ether is 400~2000.
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