CN109135504A - A kind of modified graphene oxide/aqueous epoxy resins composite coating and preparation method thereof - Google Patents
A kind of modified graphene oxide/aqueous epoxy resins composite coating and preparation method thereof Download PDFInfo
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- CN109135504A CN109135504A CN201810843347.0A CN201810843347A CN109135504A CN 109135504 A CN109135504 A CN 109135504A CN 201810843347 A CN201810843347 A CN 201810843347A CN 109135504 A CN109135504 A CN 109135504A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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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
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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
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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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
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Paints Or Removers (AREA)
Abstract
The present invention provides a kind of modified graphene oxide/aqueous epoxy resins composite coatings and preparation method thereof, are composed of the following raw materials in parts by weight: 10-20 parts of aqueous epoxy resins；20-40 parts of curing agent；30-40 parts of deionized water；0.6-1 parts of auxiliary agent；Silica/0.01-0.03 parts of graphene oxide.By with potassium water glass modified graphene oxide, so that surface of graphene oxide loads upper silica, to further promote its dispersibility in water, it is added it in aqueous epoxide resin paint system again, the defect for effectively compensating for epoxy resin itself, has devised a kind of coating haveing excellent performance.
Description
Technical field
The present invention relates to the modifications of graphene oxide, and its dispersion in water and the application field in coating, especially
It is related to a kind of modified graphene oxide/aqueous epoxy resins composite coating and preparation method thereof.
Background technique
The owned many performances outstanding of epoxy coating, including good adhesive force, excellent chemical-resistance
Deng this makes it have broad mass market in fields such as priming paint, floor paint, anti-decaying paints.But there is also certain defect, examples for epoxy resin
Such as poor weatherability, lower hardness, for aqueous epoxy resins, in film forming procedure, with waving for aqueous solvent
Hair, easily formation pin hole, this also limits its application to a certain extent.
Derivative of the graphene oxide as graphene on the basis of retaining graphene two-dimensional structure, and is grafted top
Point oxygen-containing functional group, including hydroxyl, carboxyl, epoxy group etc., this make graphene oxide have the activity bigger than graphene and
Better compatibility.Therefore, being added in coating using graphene oxide as filler, which improves paint film property, also has become a hot topic of research.
But due to the characteristics of graphene oxide layer structure, the effect of delocalized pi-bond between biggish interlayer Van der Waals force and carbon atom, then
In conjunction with the actual conditions of coating, even several months a couple of days just constructs usually after deployed, and the compatibility of current graphene oxide is also
It is insufficient for demand, so graphene oxide is modified by many people, it is found that modified graphene oxide possesses more to go out
The dispersion effect of color.
Modifying agent used at this stage is virtually all around organic matter, including silane coupling agent, p-phenylenediamine, just
Tetraethyl orthosilicate, polyisocyanate etc., not only price is higher for these reagents, it is often more important that does not meet environmentally friendly trend instantly.
Summary of the invention
In order to overcome above-mentioned deficiency, the present invention provide a kind of modified graphene oxide/aqueous epoxy resins composite coating and
Preparation method.By with potassium water glass modified graphene oxide, so that surface of graphene oxide loads upper silica, thus
Its dispersibility in water is further promoted, then is added it in aqueous epoxide resin paint system, ring is effectively compensated for
The defect of oxygen resin itself has devised a kind of coating haveing excellent performance.
To achieve the goals above, the present invention adopts the following technical scheme:
A kind of modified graphene oxide/aqueous epoxy resins composite coating, is composed of the following raw materials in parts by weight:
Wherein, silica/graphene oxide preparation process is as follows:
By graphene oxide, potassium water glass, dehydrated alcohol, deionized water mixing, ultrasonic treatment a period of time, then in room temperature
For a period of time, centrifugation, washing are dry to get silica/graphene oxide for lower mechanical mixture.
Since the big pi bond structure of graphene surface has hydrophobicity and chemical inertness, aggregation is easily stacked in epoxy coating,
Graphene is caused to be difficult to give full play to performance in epoxy matrix.For this purpose, method of the prior art by surface grafting, by graphite
Alkene and the SiO haveing excellent performance2Nanoparticle combines, and this method does not only generate destruction to the basic structure of graphene, also
The intrinsic performance characteristics of graphene are maintained, but the dispersion effect of organic silicon source modified graphene oxide is ideal not enough, also lacks
Weary systematic research generally requires addition stabilizer or carries out ultrasonic disperse.For this purpose, the application system research SiO2Nanoparticle
The combination rule of son and graphene and its influence to dispersibility, grope to find by large scale experiment: being made using potassium water glass
Traditional organic silicon source is substituted for inorganic silicon source, and SiO not only may be implemented2Effective combination of nanoparticle and graphene, meanwhile,
Potassium oxide in potassium water glass, which can provide alkaline environment, keeps the surface functional group of graphene oxide negatively charged, effectively improves graphite
The dispersibility of alkene preferably meets functionalization graphene/epoxy coating performance requirement.
In some embodiments, the silica/graphene oxide, potassium water glass, dehydrated alcohol, the matter of deionized water
Amount is than being 0.02-0.03:0.4-0.6:40-42:48-50.
In some embodiments, the ultrasonic treatment condition are as follows: 20~30min of ultrasound under 300~350W.
In some embodiments, the potassium water glass is Shandong You Suo Chemical Industry Science Co., Ltd potassium water glass (liquid silicon
Sour potassium), modulus 3.3, Baume degrees 40.
In some embodiments, the aqueous epoxy resins are Shanghai Hanzhong coating Co., Ltd 228A aqueous epoxy resins
In some embodiments, the curing agent is the solidification of Shanghai Hanzhong coating Co., Ltd 228B aqueous epoxy resins
Agent.
In some embodiments, the auxiliary agent includes: defoaming agent, wetting agent, levelling agent.
In some embodiments, the defoaming agent is BYK-021 defoaming agent,
In some embodiments, the wetting agent is BYK-348 wetting agent,
In some embodiments, the levelling agent is BYK-381 levelling agent.
The present invention also provides a kind of modified graphene oxide/aqueous epoxy resins composite coating preparation methods, comprising:
By graphene oxide, potassium water glass, dehydrated alcohol, deionized water mixing, ultrasonic treatment a period of time, then in room temperature
For a period of time, centrifugation, washing are dry for lower mechanical mixture, obtain silica/graphene oxide；
Silica/graphene oxide is taken to be distributed in water, ultrasound a period of time；
Curing agent, defoaming agent are sequentially added, is uniformly mixed；
Be added epoxy resin, water, be added dropwise wetting agent, levelling agent, be uniformly mixed, stand to get.
In some embodiments, the mass ratio of the epoxy resin, curing agent and deionized water is 1:2:3.
The present invention also provides any above-mentioned modified graphene oxide/aqueous epoxy resins composite coatings at preparation bottom
Paint, floor paint, the application in anti-decaying paint.
Beneficial effects of the present invention
(1) present invention goes to be modified graphene oxide with this cheap inorganic reagent of potassium water glass, obtains
Silica/graphene oxide of similar go structure, not only makes the dispersibility of graphene oxide have very big promotion in this way, can
It is not settled with reaching the several months；Also have very great help to the overall performance of paint film system simultaneously.
(2) modified graphene oxide of the application preparation effectively compensates for the defect of epoxy resin, the mechanicalness of paint film
Energy and antiseptic property have promotion；
(3) preparation method of the present invention is simple, film forming efficiency is high, practical, easy to spread.
Detailed description of the invention
The accompanying drawings constituting a part of this application is used to provide further understanding of the present application, and the application's shows
Meaning property embodiment and its explanation are not constituted an undue limitation on the present application for explaining the application.
Fig. 1 be embodiment 1 prepare modified graphene oxide (silica/graphene oxide) with it is unmodified in embodiment 4
Graphene oxide infrared comparative analysis as scheme
Fig. 2 is modified graphene oxide (silica/graphene oxide) prepared by embodiment 1 and does not change in embodiment 4
The dispersion comparison diagram of the graphene oxide of property.
Fig. 3 is film prepared by embodiment 1 and film pendulum-rocker hardness comparison diagram prepared by embodiment 4.
Fig. 4 is the acidproof immersion test comparison diagram 4 of film prepared with embodiment 4 that embodiment 1 prepares film.
Specific embodiment
It is noted that following detailed description is all illustrative, it is intended to provide further instruction to the application.Unless another
It indicates, all technical and scientific terms used herein has usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
This application provides a kind of coating systems, and composition is as follows, and the number is parts by weight:
Technique of the invention is as follows:
(1) a small amount of silica/graphene oxide is taken to be distributed in appropriate amount of deionized water, ultrasound 20 minutes；
(2) corresponding amount curing agent is added, then a small amount of defoaming agent is added dropwise, stirs 10 minutes, keeps curing agent hydrophilic radical abundant
Expansion；
(3) mass ratio that corresponding amount epoxy resin, epoxy resin and curing agent and deionized water is then added is 1:2:3,
The amount of water can carry out a little adjustment according to execution conditions, then a little wetting agent, levelling agent is added dropwise, and stirring after ten minutes, stands 5
Minute can construct；
Wherein silica/graphene oxide preparation process is as follows:
By graphene oxide, potassium water glass, dehydrated alcohol, deionized water is 0.02-0.03:0.4-0.6 according to mass ratio:
40:50 mixing, ultrasound 20 minutes, then be stirred at room temperature 8 hours, it is respectively washed three times after centrifugation with deionized water and dehydrated alcohol,
It is dry.Up to silica/graphene oxide.
Graphene oxide used in the following embodiment all uses Hummers method to prepare.
Epoxy resin and curing agent are purchased from Shanghai Hanzhong coating Co., Ltd, the aqueous ring of 228A aqueous epoxy resins, 228B
Oxygen resin curing agent；
Potassium water glass is purchased from Shandong You Suo Chemical Industry Science Co., Ltd；
Defoaming agent, levelling agent, wetting agent are purchased from German Bi Ke company, BYK-021 defoaming agent, BYK-348 wetting agent, BYK-
381 levelling agents.
Embodiment 1: the present invention provides a kind of modified graphene oxide/aqueous epoxide resin paint, the system by
Following component composition, the number is parts by weight:
1) silica/graphene oxide is realized according to following technique:
According to m graphene oxide: m potassium water glass: m dehydrated alcohol: m deionized water=0.02:0.4:40:50 mixing surpasses
Sound 20 minutes, then be stirred at room temperature 8 hours, it is respectively washed three times after centrifugation with deionized water and dehydrated alcohol, it is dry.Up to dioxy
SiClx/graphene oxide.
2) film the specific process is as follows:
(1) silica/graphene oxide is distributed in appropriate amount of deionized water, ultrasound 20 minutes；
(2) corresponding amount curing agent is added, then a small amount of defoaming agent (curing agent: defoaming agent=100:1) is added dropwise, stirs 10 points
Clock is sufficiently spread out curing agent hydrophilic radical；
(3) mass ratio that corresponding amount epoxy resin, epoxy resin and curing agent and deionized water is then added is 1:2:3,
A little wetting agent, levelling agent (defoaming agent: wetting agent: levelling agent=1:1:1) are added dropwise again, stirring after ten minutes, stands 5 minutes i.e.
It can construct；
Embodiment 2: the present invention provides a kind of modified graphene oxide/aqueous epoxide resin paint, the system by
Following component composition, the number is parts by weight:
1) silica/graphene oxide is realized according to following technique:
According to m graphene oxide: m potassium water glass: m dehydrated alcohol: m deionized water=0.025:0.5:40:50 mixing surpasses
Sound 20 minutes, then be stirred at room temperature 8 hours, it is respectively washed three times after centrifugation with deionized water and dehydrated alcohol, it is dry.Up to dioxy
SiClx/graphene oxide.
2) film the specific process is as follows:
(1) silica/graphene oxide is distributed in appropriate amount of deionized water, ultrasound 20 minutes；
(2) corresponding amount curing agent is added, then a small amount of defoaming agent is added dropwise, stirs 10 minutes, keeps curing agent hydrophilic radical abundant
Expansion；
(3) mass ratio that corresponding amount epoxy resin, epoxy resin and curing agent and deionized water is then added is 1:2:3,
A little wetting agent, levelling agent are added dropwise again, after ten minutes, standing 5 minutes can construct for stirring；
Embodiment 3: described the present invention provides the modified graphene oxide/aqueous epoxide resin paint haveing excellent performance
System is made of the following components, and the number is parts by weight:
1) silica/graphene oxide is realized according to following technique:
According to m graphene oxide: m potassium water glass: m dehydrated alcohol: m deionized water=0.03:0.6:40:50 mixing surpasses
Sound 20 minutes, then be stirred at room temperature 8 hours, it is respectively washed three times after centrifugation with deionized water and dehydrated alcohol, it is dry.Up to dioxy
SiClx/graphene oxide.
2) film the specific process is as follows:
(1) silica/graphene oxide is distributed in appropriate amount of deionized water, ultrasound 20 minutes；
(2) corresponding amount curing agent is added, then a small amount of defoaming agent is added dropwise, stirs 10 minutes, keeps curing agent hydrophilic radical abundant
Expansion；
(3) mass ratio that corresponding amount epoxy resin, epoxy resin and curing agent and deionized water is then added is 1:2:3,
A little wetting agent, levelling agent are added dropwise again, after ten minutes, standing 5 minutes can construct for stirring；
Silica/the graphene oxide is realized according to following technique:
According to m graphene oxide: m potassium water glass: m dehydrated alcohol: m deionized water=0.03:0.6:40:50 mixing surpasses
Sound 20 minutes, then be stirred at room temperature 8 hours, it is respectively washed three times after centrifugation with deionized water and dehydrated alcohol, it is dry.Up to dioxy
SiClx/graphene oxide.
Embodiment 4: the present invention provides the silica/graphene oxide/aqueous epoxide resin paint haveing excellent performance, institutes
The system stated is made of the following components, and the number is parts by weight:
Film the specific process is as follows:
(1) graphene oxide is distributed in appropriate amount of deionized water, ultrasound 20 minutes；
(2) corresponding amount curing agent is added, then a small amount of defoaming agent (curing agent: defoaming agent=100:1) is added dropwise, stirs 10 points
Clock is sufficiently spread out curing agent hydrophilic radical；
(3) mass ratio that corresponding amount epoxy resin, epoxy resin and curing agent and deionized water is then added is 1:2:3,
A little wetting agent, levelling agent (defoaming agent: wetting agent: levelling agent=1:1:1) are added dropwise again, stirring after ten minutes, stands 5 minutes i.e.
It can construct；
Embodiment 5
To in above-described embodiment 1,4, modified graphene oxide (silica/graphene oxide) and graphene oxide, and
The performance of its corresponding film prepared is compared.
Wherein, embodiment 1 prepare modified graphene oxide (silica/graphene oxide) with it is unmodified in embodiment 4
Graphene oxide infrared comparative analysis it is as shown in Figure 1.Infrared test instrument is Fourier infrared spectrograph (Bruker
Vector22), test condition is tabletting test.
The dispersion pair of unmodified graphene oxide in silica/graphene oxide and embodiment 4 prepared by embodiment 1
Than as shown in Figure 2.Test method are as follows: 0.05mg silica/graphene oxide is distributed in 15mL water, it is ultrasonic under 300W
20min。
Film pendulum-rocker hardness comparison prepared by film and embodiment 4 prepared by embodiment 1 is as shown in Figure 3.Test method are as follows:
The paint brush prepared is coated on the glass plate of 120*90*3mm, tests pendulum-rocker hardness after paint film is done solid work.
The acidproof immersion test comparison of the film prepared with embodiment 4 that embodiment 1 prepares film is as shown in Figure 4.Test side
Method are as follows: the paint brush prepared is coated on the tinplate of 120*50*0.28mm, being immersed in mass fraction after paint film is done solid work is
In 10% hydrochloric acid, phenomenon is observed.
The foregoing is merely preferred embodiment of the present application, are not intended to limit this application, for the skill of this field
For art personnel, various changes and changes are possible in this application.Within the spirit and principles of this application, made any to repair
Change, equivalent replacement, improvement etc., should be included within the scope of protection of this application.
Claims (10)
1. a kind of modified graphene oxide/aqueous epoxy resins composite coating, which is characterized in that by the raw material group of following parts by weight
At:
Wherein, silica/graphene oxide preparation process is as follows:
By graphene oxide, potassium water glass, dehydrated alcohol, deionized water mixing, ultrasonic treatment a period of time, then machine at room temperature
Tool mixing a period of time, centrifugation, washing are dry to get silica/graphene oxide.
2. coating as described in claim 1, which is characterized in that the graphene oxide, potassium water glass, dehydrated alcohol, go from
The mass ratio of sub- water is 0.02-0.03:0.4-0.6:40-42:48-50.
3. coating as described in claim 1, which is characterized in that the ultrasonic treatment condition are as follows: ultrasound 20- under 300-350W
30min。
4. coating as described in claim 1, which is characterized in that the modulus of the potassium water glass is 3.3, Baume degrees 40.
5. coating as described in claim 1, which is characterized in that the curing agent is aqueous epoxy resin curing agent.
6. coating as described in claim 1, which is characterized in that the auxiliary agent includes: defoaming agent, wetting agent, levelling agent.
7. coating as described in claim 1, which is characterized in that the defoaming agent is BYK-021 defoaming agent,
The wetting agent is BYK-348 wetting agent, and the levelling agent is BYK-381 levelling agent.
8. a kind of modified graphene oxide/aqueous epoxy resins composite coating preparation method characterized by comprising
By graphene oxide, potassium water glass, dehydrated alcohol, deionized water mixing, ultrasonic treatment a period of time, then machine at room temperature
Tool mixing a period of time, centrifugation, washing are dry, obtain silica/graphene oxide；
Silica/graphene oxide is taken to be distributed in water, ultrasound a period of time；
Curing agent, defoaming agent are sequentially added, is uniformly mixed；
Be added epoxy resin, water, be added dropwise wetting agent, levelling agent, be uniformly mixed, stand to get.
9. method according to claim 8, which is characterized in that the mass ratio of the epoxy resin, curing agent and deionized water
For 1:2:3.
10. the described in any item modified graphene oxides of claim 1-7/aqueous epoxy resins composite coating prepare priming paint,
Application in floor paint, anti-decaying paint.
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| CN201810843347.0A CN109135504B (en) | 2018-07-27 | 2018-07-27 | A kind of modified graphene oxide/aqueous epoxy resins composite coating and preparation method thereof |
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| CN114804648A (en) * | 2022-03-29 | 2022-07-29 | 中国科学院福建物质结构研究所 | Fluorine-free self-cleaning coating and preparation method and application thereof |
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| CN109135504B (en) | 2019-08-23 |
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