CN108727962A - A kind of aqueous polyurethane coating and graphene oxide composite coating interface ultrabranching polyamide adhering method - Google Patents
A kind of aqueous polyurethane coating and graphene oxide composite coating interface ultrabranching polyamide adhering method Download PDFInfo
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- CN108727962A CN108727962A CN201810674017.3A CN201810674017A CN108727962A CN 108727962 A CN108727962 A CN 108727962A CN 201810674017 A CN201810674017 A CN 201810674017A CN 108727962 A CN108727962 A CN 108727962A
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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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/001—Macromolecular compounds containing organic and inorganic sequences, e.g. organic polymers grafted onto silica
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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
- C09D7/65—Additives macromolecular
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Abstract
The invention discloses a kind of aqueous polyurethane coatings and graphene oxide composite coating interface ultrabranching polyamide adhering method.Situ-formed graft is realized in the polycondensation reaction that carboxyl of this method based on surface of graphene oxide participates in ultrabranching polyamide, obtain the graphene oxide of situ-formed graft ultrabranching polyamide, the amido for further utilizing ultrabranching polyamide molecular end abundant participates in the solidification of aqueous polyurethane coating, realizes that aqueous polyurethane coating is bonding with graphene oxide.On the one hand graphene oxide grafting ultrabranching polyamide improves the dispersion performance of graphene oxide, on the other hand interfacial chemical reaction is improved, the adhering method improves the mechanical property and water resistance of coating, there is extensive market application prospect, has good economic benefit and social benefit.
Description
Technical field
The present invention relates to aqueous polyurethane coatings and graphene oxide composite coating bonding interface method, belong to aqueous poly- ammonia
Ester composite coating interface processing field.
Background technology
Polyurethane refers to the polymer containing carbamate groups, referred to as polyurethanes in macromolecular main chain, due to
The group contained in polyurethane macromolecular is all highly polar group, and also contains polyethers or polyester flexible segment in macromolecular,
So that polyurethane has higher mechanical strength and an oxidation stability, higher flexibility and resilience are excellent oil resistivity, resistance to
Solvent borne, water resistance and fire resistance, are widely used in coating and adhesive etc..Recent years, with people's environmental consciousness
Gradually reinforcement, environmentally friendly water-base resin become research hot spot.Aqueous polyurethane coating is with aqueous polyurethane tree
Fat is base-material and using water as a kind of coating of decentralized medium, and comprehensive performance is preferable, safety and environmental protection, in coating, adhesive, oil
The fields such as ink, sealant and surface conditioning agent obtain increasingly extensive application.But the mechanical property of its latex film (intensity, mould
Amount), chemical resistance etc. can't compare favourably with traditional solvent borne polyurethane, thus limit aqueous polyurethane into one
Walk extensive use.
By organic resin and inorganic material such as silica, clay etc. can effectively improve polyurethane film modulus,
Tensile strength, hardness, wearability etc. and water-fast and mechanical property.Graphene has nano-lamellar structure, to improving aqueous poly- ammonia
The anti-dielectric behavior of ester oxygen coating has great importance.The surface modifying method of graphene oxide disperses to it and and polyurethane
Reactivity be research emphasis, become the key that aqueous polyurethane coating and graphene composite coating improve.Currently, oxygen
Graphite alkene process for modifying surface method is there are clearly disadvantageous, and specific aim is not strong and effect is not notable.It is proposed by the present invention
Situ-formed graft has the ultrabranching polyamide of height unique branched structure and functional end-group, is to realize graphene oxide in water
Property polyurethane coating in high uniformity dispersion and high bonding key.
Invention content
For overcome the deficiencies in the prior art, a kind of aqueous polyurethane coating of present invention offer and the compound painting of graphene oxide
Bed boundary ultrabranching polyamide adhering method realizes that graphene oxide high uniformity dispersion and height in aqueous polyurethane coating are viscous
It connects.
In order to achieve the above-mentioned object of the invention, the technical solution adopted by the present invention is：A kind of aqueous polyurethane coating and oxidation
Graphene composite coating interface ultrabranching polyamide adhering method, it is characterised in that：It is aqueous poly- ammonia using ultrabranching polyamide
Interface bonding agent between ester and graphene oxide, including dispersion steps of the graphene oxide in polyamines based compound, oxidation
The step of graphene situ-formed graft ultrabranching polyamide, situ-formed graft ultrabranching polyamide graphene oxide and aqueous polyurethane
The bonding interface reaction step of coating.
Surface of graphene oxide contains enough carboxylic acid groups, and carboxylic acid is enable to react to form amide groups with amino.If carboxylic
Acid groups, which do not reach requirement, needs further oxidation processes.
In the step of graphene oxide situ-formed graft ultrabranching polyamide, acid anhydrides is added, acid anhydrides is succinic anhydride, adjacent benzene two
The mixture of formic anhydride or both.
In dispersion steps of the graphene oxide in polyamines based compound, the polyamines for being used to prepare ultrabranching polyamide is official
Low molecular compound and its mixture that quantity is not less than 3 can be rolled into a ball.Polyamines based compound is the polyamines, it is preferable that polyamines
For the mixture of diethylenetriamine, polyethylene polyamine or both.
In dispersion steps of the graphene oxide in polyamines based compound, using ultrasonic disperse equipment.
In the step of graphene oxide situ-formed graft ultrabranching polyamide, in point of graphene oxide and polyamines based compound
The mixture of a certain amount of succinic anhydride or phthalic anhydride or both is added in granular media system, stirs evenly, is warming up to 120-135
Degree Celsius, keep the temperature 2-4 hours（It is preferred that 3 hours）It carries out that reactant is obtained by the reaction, cools to 70-90 DEG C.
For the ultrabranching polyamide for removing non-grafted, waits for that reactant cools to 70-90 degrees Celsius, be dissolved in water non-grafted
Ultrabranching polyamide centrifuges the ultrabranching polyamide graphene oxide for obtaining situ-formed graft, further washes, finally will be former
The ultrabranching polyamide graphene oxide of position grafting is diluted to a certain concentration, spare.
When aqueous polyurethane coating is reacted with graphene oxide progress bonding interface, by certain aqueous polyurethane dispersion
It is uniformly mixed, the ultrabranching polyamide graphene oxide of 0.1 ~ 2% situ-formed graft is added, aqueous polyurethane coating is obtained after solidification
Coating.
Aqueous polyurethane coating and graphene oxide composite coating interface ultrabranching polyamide adhering method, feature exist
In：The specific steps are：Take graphene oxide and polyamines, ultrasonic disperse -1 hour 20 minutes, wherein graphene oxide and polyamines
Mass ratio is 1:9-1:15；The dispersion of graphene oxide and polyamines is added in the flask equipped with blender, then is slowly added
Enter acid anhydrides, the mass ratio of acid anhydrides and polyamines is：1：1-2 reacts 1 hour at 50 DEG C -55 DEG C, leads to nitrogen protection, stops stirring, rises
Temperature carries out melt polycondensation reaction 3 hours or more to 120-135 degrees Celsius, cools to 90 DEG C, water is added to form the over-expense of situ-formed graft
Change polyamide graphene oxide dispersion, centrifuge, washing configures the graphene oxide of situ-formed graft ultrabranching polyamide
1%（Mass ratio）The graphene oxide dispersion of the situ-formed graft ultrabranching polyamide of concentration, it is spare；Then, a certain amount of water is weighed
Property polyurethane, add mass ratio 0.1 ~ 2% grafting ultrabranching polyamide graphene oxide dispersion, stir evenly, spray
It applies, it is dry complete.（Note：Mass ratio 0.1 ~ 2% refers to that the graphene oxide of grafting ultrabranching polyamide accounts for grafting hyperbranched poly
The mass ratio of the graphene oxide dispersion of amide, the gross mass of aqueous polyurethane.）
Compared with the existing technology, the present invention realizes following advantageous effect：By the carboxyl of surface of graphene oxide participate in polyamines with
Acid anhydrides prepares the polycondensation reaction of ultrabranching polyamide, obtains graphene oxide situ-formed graft ultrabranching polyamide, further utilizes
The abundant amido of ultrabranching polyamide molecular end participates in the solidification of aqueous polyurethane coating, realizes aqueous polyurethane coating and oxygen
The bonding of graphite alkene.On the one hand the dispersion performance for improving graphene oxide, on the other hand improves interfacial chemical reaction, should
Adhering method improves the mechanics and water resistance of coating.
Specific implementation mode
For a better understanding of the present invention, below with specific example come the technical solution that the present invention will be described in detail, but this
Invention is not limited thereto.
Embodiment 1
First, 10 grams of graphene oxides and 104 grams of diethylenetriamines are taken to be uniformly mixed, dress is added in ultrasonic disperse 20 minutes or more
Have in the three-necked flask of blender, be slowly added to 100 grams of succinic anhydrides, reacted 1 hour at 50 DEG C or so, leads to nitrogen protection, stop
It only stirs, is warming up to 130 degree of melt polycondensation reactions 3 hours or more, cools to 90 DEG C or so, water is added to proceed to form black dispersion
Liquid centrifuges, washing, and the graphene oxide of situ-formed graft ultrabranching polyamide is configured 1%（Mass ratio）The dispersion of concentration
Liquid, it is spare.Then, a certain amount of aqueous polyurethane is weighed, the graphene oxide that mass ratio 0.2% is grafted ultrabranching polyamide is added
Dispersion liquid stirs evenly, spraying, dry completely rear test performance.Before ultrabranching polyamide being grafted compared to graphene oxide, oxidation
The dispersion performance of graphene significantly improves, and enhances with the bonding interface of aqueous polyurethane, the water-fast and mechanical property of coating is notable
It improves, paint film water absorption rate is reduced is reduced to 13% by 18%, and tensile strength is increased to 24MPa by 22MPa.
Embodiment 2
First, 10 grams of graphene oxides and 146 grams of polyethylene polyamines are taken to be uniformly mixed, dress is added in ultrasonic disperse 20 minutes or more
Have in the three-necked flask of blender, be slowly added to 100 grams of succinic anhydrides, reacted 1 hour at 50 DEG C or so, leads to nitrogen protection, stop
It only stirs, is warming up to 130 degree of melt polycondensation reactions 3 hours or more, cools to 90 DEG C or so, water is added to proceed to form black dispersion
Liquid centrifuges, washing, and the graphene oxide of situ-formed graft ultrabranching polyamide is configured 1%（Mass ratio）The dispersion of concentration
Liquid, it is spare.Then, example weighs aqueous polyurethane according to a certain ratio, and the oxidation that mass ratio 0.5% is grafted ultrabranching polyamide is added
Graphene dispersing solution stirs evenly, spraying, dry completely rear test performance.It is grafted ultrabranching polyamide compared to graphene oxide
Before, the dispersion performance of graphene oxide significantly improves, and enhances with the bonding interface of aqueous polyurethane, the water-fast and mechanical property of coating
It can significantly improve, paint film water absorption rate is reduced is reduced to 14% by 18%, and tensile strength is increased to 25MPa by 22MPa.
Embodiment 3
First, 10 grams of graphene oxides and 104 grams of diethylenetriamines are taken to be uniformly mixed, dress is added in ultrasonic disperse 20 minutes or more
Have in the three-necked flask of blender, be slowly added to 148 grams of phthalic anhydrides, reacted 1 hour at 50 DEG C or so, leads to nitrogen and protect
Shield stops stirring, is warming up to 130 degree of melt polycondensation reactions 3 hours or more, cools to 90 DEG C or so, add water proceed to be formed it is black
Color dispersion liquid centrifuges, washing, and the graphene oxide of situ-formed graft ultrabranching polyamide is configured 1%（Mass ratio）Concentration
Dispersion liquid, it is spare.Then, example weighs aqueous polyurethane according to a certain ratio, and mass ratio 0.5% is added and is grafted ultrabranching polyamide
Graphene oxide dispersion stirs evenly, spraying, dry completely rear test performance.It is grafted hyperbranched poly compared to graphene oxide
Before amide, the dispersion performance of graphene oxide significantly improves, and enhances with the bonding interface of aqueous polyurethane, the water-fast and power of coating
It learns performance to significantly improve, paint film water absorption rate is reduced is reduced to 13% by 18%, and tensile strength is increased to 25MPa by 22MPa.
Embodiment 4
First, 10 grams of graphene oxides and 146 grams of polyethylene polyamines are taken to be uniformly mixed, dress is added in ultrasonic disperse 20 minutes or more
Have in the three-necked flask of blender, be slowly added to 100 grams of succinic anhydrides, reacted 1 hour at 50 DEG C or so, leads to nitrogen protection, stop
It only stirs, is warming up to 130 degree of melt polycondensation reactions 3 hours or more, cools to 90 DEG C or so, water is added to proceed to form black dispersion
Liquid centrifuges, washing, and the graphene oxide of situ-formed graft ultrabranching polyamide is configured 1%（Mass ratio）The dispersion of concentration
Liquid, it is spare.Then, example weighs aqueous polyurethane according to a certain ratio, and the oxidation that mass ratio 0.2% is grafted ultrabranching polyamide is added
Graphene dispersing solution stirs evenly, spraying, dry completely rear test performance.It is grafted ultrabranching polyamide compared to graphene oxide
Before, the dispersion performance of graphene oxide significantly improves, and enhances with the bonding interface of aqueous polyurethane, the water-fast and mechanical property of coating
It can significantly improve, paint film water absorption rate is reduced is reduced to 14% by 18%, and tensile strength is increased to 26MPa by 22MPa.
Embodiment 5
First, 10 grams of graphene oxides and 104 grams of diethylenetriamines are taken to be uniformly mixed, dress is added in ultrasonic disperse 20 minutes or more
Have in the three-necked flask of blender, be slowly added to 100 grams of succinic anhydrides, reacted 1 hour at 50 DEG C or so, leads to nitrogen protection, stop
It only stirs, is warming up to 130 degree of melt polycondensation reactions 3 hours or more, cools to 90 DEG C or so, water is added to proceed to form black dispersion
Liquid centrifuges, washing, and the graphene oxide of situ-formed graft ultrabranching polyamide is configured 1%（Mass ratio）The dispersion of concentration
Liquid, it is spare.Then, example weighs aqueous polyurethane according to a certain ratio, and the oxidation that mass ratio 0.6% is grafted ultrabranching polyamide is added
Graphene dispersing solution stirs evenly, spraying, dry completely rear test performance.It is grafted ultrabranching polyamide compared to graphene oxide
Before, the dispersion performance of graphene oxide significantly improves, and enhances with the bonding interface of aqueous polyurethane, the water-fast and mechanical property of coating
It can significantly improve, paint film water absorption rate is reduced is reduced to 15% by 18%, and tensile strength is increased to 26MPa by 22MPa.
Embodiment 6
First, 10 grams of graphene oxides and 104 grams of diethylenetriamines are taken to be uniformly mixed, dress is added in ultrasonic disperse 20 minutes or more
Have in the three-necked flask of blender, be slowly added to 50 grams of succinic anhydrides and 50 grams of phthalic anhydrides, it is small that 1 is reacted at 50 DEG C or so
When, lead to nitrogen protection, stop stirring, be warming up to 130 degree of melt polycondensation reactions 3 hours or more, cool to 90 DEG C or so, add water after
Continue to black dispersion liquid is formed, centrifuge, the graphene oxide of situ-formed graft ultrabranching polyamide is configured 1% by washing（Matter
Amount ratio）The dispersion liquid of concentration, it is spare.Then, example weighs aqueous polyurethane according to a certain ratio, and the grafting over-expense of mass ratio 0.8% is added
The graphene oxide dispersion for changing polyamide, stirs evenly, and sprays, dry completely rear test performance.It is connect compared to graphene oxide
Before branch ultrabranching polyamide, the dispersion performance of graphene oxide significantly improves, and enhances with the bonding interface of aqueous polyurethane, coating
Water-fast and mechanical property significantly improve, paint film water absorption rate is reduced is reduced to 12% by 18%, and tensile strength is increased to by 22MPa
26MPa。
The above display describes the basic principles and main features and advantage of the present invention.The technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, what is described in the above embodiment and the description is only saying the principle of the present invention,
Without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes and improvements are all
It drops into the claimed scope of the invention.The scope of the present invention is defined by the appended claims and its equivalents.
Claims (10)
1. a kind of aqueous polyurethane coating and graphene oxide composite coating interface ultrabranching polyamide adhering method, feature exist
In：Existed using interface bonding agent of the ultrabranching polyamide between aqueous polyurethane and graphene oxide, including graphene oxide
The step of dispersion steps in polyamines based compound, graphene oxide situ-formed graft ultrabranching polyamide, situ-formed graft are hyperbranched
The graphene oxide of polyamide and the bonding interface reaction step of aqueous polyurethane coating.
2. a kind of aqueous polyurethane coating according to claim 1 and the hyperbranched polyamides in graphene oxide composite coating interface
Amine adhering method, it is characterised in that：Surface of graphene oxide contains enough carboxylic acid groups, and carboxylic acid is enable to react to be formed with amino
Amide groups.
3. a kind of aqueous polyurethane coating according to claim 1 and the hyperbranched polyamides in graphene oxide composite coating interface
Amine adhering method, it is characterised in that：In the step of graphene oxide situ-formed graft ultrabranching polyamide, acid anhydrides is added, acid anhydrides is
Succinic anhydride, the mixture of phthalic anhydride or both.
4. a kind of aqueous polyurethane coating according to claim 1 and the hyperbranched polyamides in graphene oxide composite coating interface
Amine adhering method, it is characterised in that：In dispersion steps of the graphene oxide in polyamines based compound, it is used to prepare hyperbranched poly
The polyamines of amide is the low molecular compound and its mixture that number of functional groups is not less than 3.
5. a kind of aqueous polyurethane coating according to claim 4 and the hyperbranched polyamides in graphene oxide composite coating interface
Amine adhering method, it is characterised in that：Polyamines based compound be the polyamines, polyamines be diethylenetriamine, polyethylene polyamine or
The mixture of the two.
6. a kind of aqueous polyurethane coating according to claim 1 and the hyperbranched polyamides in graphene oxide composite coating interface
Amine adhering method, it is characterised in that：In dispersion steps of the graphene oxide in polyamines based compound, set using ultrasonic disperse
It is standby.
7. a kind of aqueous polyurethane coating according to claim 1 and the hyperbranched polyamides in graphene oxide composite coating interface
Amine adhering method, it is characterised in that：In the step of graphene oxide situ-formed graft ultrabranching polyamide, in graphene oxide and more
The mixture of a certain amount of succinic anhydride or phthalic anhydride or both is added in the dispersion of amine compound, stirring is equal
It is even, it is warming up to 120-135 degrees Celsius, heat preservation carries out that reactant is obtained by the reaction for 2-4 hours, cools to 70 DEG C ~ 90 DEG C.
8. a kind of aqueous polyurethane coating according to claim 1 and the hyperbranched polyamides in graphene oxide composite coating interface
Amine adhering method, it is characterised in that：For the ultrabranching polyamide for removing non-grafted, waits for that reactant cools to 70-90 degrees Celsius, add
The non-grafted ultrabranching polyamide of water dissolution centrifuges the graphene oxide for obtaining situ-formed graft ultrabranching polyamide, into one
Step washing, is finally diluted to a certain concentration by the graphene oxide of situ-formed graft ultrabranching polyamide, spare.
9. a kind of aqueous polyurethane coating according to claim 1 and the hyperbranched polyamides in graphene oxide composite coating interface
Amine adhering method, it is characterised in that：When aqueous polyurethane coating is reacted with graphene oxide progress bonding interface, by certain water
Property dispersions of polyurethanes be uniformly mixed, be added 0.1 ~ 2% situ-formed graft ultrabranching polyamide graphene oxide, obtained after solidification
Aqueous polyurethane coating coating.
10. a kind of aqueous polyurethane coating according to claim 1 and graphene oxide composite coating interface hyperbranched poly
Amide adhering method, it is characterised in that：The specific steps are：Take graphene oxide and polyamines, ultrasonic disperse -1 hour 20 minutes,
The mass ratio of middle graphene oxide and polyamines is 1:9-1:15；The dispersion of graphene oxide and polyamines is added equipped with stirring
In the flask of device, it is slow added into acid anhydrides, the mass ratio of acid anhydrides and polyamines is：1：1-2 reacts 1-2 hours at 50 DEG C -55 DEG C,
Logical nitrogen protection, stops stirring, is warming up to 120-135 degrees Celsius and carries out melt polycondensation reaction 2 ~ 4 hours, cools to 70 DEG C ~ 90
DEG C, add water to form the ultrabranching polyamide graphene oxide dispersion of situ-formed graft, centrifuge, washing surpasses situ-formed graft
The graphene oxide dispersion of the situ-formed graft ultrabranching polyamide of the graphene oxide configuration 1% of branched polyamide, it is spare, 1%
The mass ratio of dispersion liquid is accounted for for the graphene oxide of situ-formed graft ultrabranching polyamide；Then, a certain amount of aqueous polyurethane is weighed,
The graphene oxide dispersion for adding the grafting ultrabranching polyamide of mass ratio 0.1 ~ 2%, stirs evenly, sprays, dried
Entirely；Mass ratio 0.1 ~ 2% refers to that the graphene oxide of grafting ultrabranching polyamide accounts for the graphite oxide of grafting ultrabranching polyamide
The mass ratio of the gross mass of alkene dispersion liquid, aqueous polyurethane.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112457763A (en) * | 2020-10-16 | 2021-03-09 | 德华兔宝宝装饰新材股份有限公司 | Preparation method and application of graphene modified polyurethane acrylate coating |
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