CN110157274A - A kind of graphene polymer water-repellent paint masterbatch and preparation method - Google Patents
A kind of graphene polymer water-repellent paint masterbatch and preparation method Download PDFInfo
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- CN110157274A CN110157274A CN201810263523.3A CN201810263523A CN110157274A CN 110157274 A CN110157274 A CN 110157274A CN 201810263523 A CN201810263523 A CN 201810263523A CN 110157274 A CN110157274 A CN 110157274A
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Classifications
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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
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
- C09D133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09D133/08—Homopolymers or copolymers of acrylic acid esters
-
- 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
-
- 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
-
- 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
-
- 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
Abstract
The present invention relates to a kind of graphene polymer water-repellent paint masterbatch and preparation method thereof, graphene/carrier including 1 parts by weight, 0.5-1 parts by weight Emulsifier, 20-30 parts by weight of polypropylene acid esters, preparation method are as follows: high concentration graphene solution preparation；Graphene/carrier solution preparation；Graphene/support powder preparation；The preparation of graphene polymer masterbatch.High production efficiency of the present invention, high-intensitive acid is not needed, production process is easy to control, and the concentration of the graphene of preparation is high, graphene/carrier of preparation, graphene can be made effectively to be wrapped on carrier, the carrier for being enclosed with graphene is sufficiently combined with polymer, play the effect of graphene high surface energy, the mechanical property of reinforced polymers film, graphene itself have hydrophobic and lyophobic property again, can prevent the infiltration of water and corrosivity organic matter, the corrosion rate for delaying paint film, plays the role of waterproof anti-corrosion.
Description
Technical field
The present invention relates to polymer waterproof coating material technical fields, and in particular to a kind of graphene polymer water-repellent paint masterbatch
And preparation method.
Background technique
Asphalt waterproofing paint is the solvent type or water-emulsifying type waterproof coatings configured using pitch as base-material, solvent type asphalt waterproofing
Coating, which refers to, to be directly dissolved in unmodified asphalt in gasoline equal solvent and is configured to, also known as adhesive bitument primer.Water and milk
Type asphalt waterproofing paint refers to asphalt under chemical emulsifier or the effect of mineral emulsifier, is dispersed in water, is formed steady
The coating that fixed aqueous dispersion is constituted.But the volatilization of pitch base waterproof coating is slow, the gas of volatilization prevents body nocuousness indoors
Water generally uses polymer waterproof coating material.
Polymer waterproof coating material has flexibility, and accurate water-proof function, referred to as builds at present, especially indoor waterproof
First choice, the waterproof principle is polymer emulsion polymerization film formation, therefore the durability of polymer film, impervious extremely important, but
It is since polymer film forming is usually together with the overbased materials such as cement, over time, polymer film is inevitable
Aging, and be difficult to repair.
And graphene is as a kind of emerging nano material, has a large specific surface area, good conductivity, chemical stability is strong,
The advantages that mechanical property and excellent thermal conductivity, electronics, optics, magnetics, in terms of have excellent performance, graphene
Also have very important significance in high-intensitive paint field, theoretically, specific surface area is high, after adding in coating, will form netted
Structure significantly enhances the caking property of coating, keeps paint film more stable.But graphene solution concentration is low at present, Bu Nengyou
Effect is distributed in polymer.
Summary of the invention
To overcome the deficiency, the purpose of the present invention is to provide a kind of graphene polymer water-repellent paint masterbatch and preparations
Method.
The technical solution adopted by the present invention to solve the technical problems is: a kind of graphene polymer water-repellent paint masterbatch,
Graphene/carrier including 1 parts by weight, 0.5-1 parts by weight Emulsifier, 20-30 parts by weight of polypropylene acid esters.
Specifically, the mass ratio of the graphene and carrier is 1:(20-30).
Preparation method are as follows:
Step 1: prepared by high concentration graphene solution
The high-purity natural crystalline flake graphite of 100mg80 mesh is weighed in 250mL polytetrafluoroethylene (PTFE) autoclave, the N methyl of 100mL is added
Pyrrolidones (NMP) organic solvent, 140-160 DEG C of reaction 3-5h, obtained graphite dispersing solution is poured into Ultrasound Instrument, setting
Certain ultrasonic power, ultrasound are taken out after a certain period of time；
Step 2: graphene/carrier solution preparation
The poromerics carrier of 2000-3000mg is added in graphite dispersing solution obtained in step 1, in turning for 2000r/min
Under speed, it is centrifuged 30min, takes upper liquid up to graphene/carrier solution, the graphene generated under high-speed rotation is wrapped in micropore
Outside material；
Step 3: graphene/support powder preparation
Graphene/carrier solution obtained in step 2 filters the NMP in removal graphene/carrier solution using cellulose membrane,
Cleaned three times with deionized water, then graphene/carrier granular be placed in the deionized water of 100mL, ultrasound obtain graphene/
Graphene/support powder is made by being freeze-dried in carrier aqueous solution.
Step 4: prepared by graphene polymer masterbatch
By the polypropylene of graphene/support powder obtained in step 3 and the emulsifier of 0.5-1 parts by weight, 20-30 parts by weight
Acid esters lotion, dispersion and emulsion 0.5h, graphene/carrier are dispersed in polyacrylate cream in the form of protomere under high velocity agitation
In liquid, a kind of high concentration graphene polymer waterproof coating material masterbatch is obtained.
Specifically, the poromerics carrier select porous carbon, diatomite, zeolite powder, in aerosil extremely
Few one kind, poromerics diameter of carrier are less than 20um.
Specifically, the emulsifier is selected from one of 0P-10, AEO-9.
Specifically, the solid content of the polyacrylate dispersion is 25-35%.
The invention has the following advantages: high production efficiency, does not need high-intensitive acid, production process is easy to control, and
The concentration of the graphene of preparation is high, and graphene/carrier of preparation can be such that graphene is effectively wrapped on carrier, be enclosed with
The carrier of graphene is sufficiently combined with polymer, the effect of performance graphene high surface energy, the mechanical property of reinforced polymers film,
Graphene itself has hydrophobic and lyophobic property again, can prevent the infiltration of water and corrosivity organic matter, delay the corrosion rate of paint film,
Play the role of waterproof anti-corrosion.
Specific embodiment
The present invention is described in further detail now.
Embodiment one
A kind of graphene polymer water-repellent paint masterbatch, graphene/carrier including 1 parts by weight, 0.5 parts by weight Emulsifier, 20
Parts by weight of polypropylene acid esters.
Preparation method are as follows:
Step 1: prepared by high concentration graphene solution
The high-purity natural crystalline flake graphite of 100mg80 mesh is weighed in 250mL polytetrafluoroethylene (PTFE) autoclave, the N methyl of 100mL is added
Pyrrolidones (NMP) organic solvent, 140-160 DEG C of reaction 3-5h, obtained graphite dispersing solution is poured into Ultrasound Instrument, setting
Certain ultrasonic power, ultrasound are taken out after a certain period of time；
Step 2: graphene/carrier solution preparation
The poromerics carrier of 2000mg is added in graphite dispersing solution obtained in step 1, under the revolving speed of 2000r/min,
It is centrifuged 30min, takes upper liquid up to graphene/carrier solution, the graphene generated under high-speed rotation is wrapped in poromerics
Outside；
Step 3: graphene/support powder preparation
Graphene/carrier solution obtained in step 2 filters the NMP in removal graphene/carrier solution using cellulose membrane,
Cleaned three times with deionized water, then graphene/carrier granular be placed in the deionized water of 100mL, ultrasound obtain graphene/
Graphene/support powder is made by being freeze-dried in carrier aqueous solution.
Step 4: prepared by graphene polymer masterbatch
By the polyacrylate cream of graphene/support powder obtained in step 3 and the emulsifier of 0.5 parts by weight, 20 parts by weight
Liquid, dispersion and emulsion 0.5h, graphene/carrier are dispersed in polyacrylate dispersion in the form of protomere under high velocity agitation,
Obtain a kind of high concentration graphene polymer waterproof coating material masterbatch.
Specifically, the poromerics carrier select porous carbon, diatomite, zeolite powder, in aerosil extremely
Few one kind, poromerics diameter of carrier are less than 20um.
Specifically, the emulsifier selects AEO-9.
Specifically, the solid content of the polyacrylate dispersion is 25-35%.
Embodiment two
A kind of graphene polymer water-repellent paint masterbatch, graphene/carrier including 1 parts by weight, 0.7 parts by weight Emulsifier, 25
Parts by weight of polypropylene acid esters.
Preparation method are as follows:
Step 1: prepared by high concentration graphene solution
The high-purity natural crystalline flake graphite of 100mg80 mesh is weighed in 250mL polytetrafluoroethylene (PTFE) autoclave, the N methyl of 100mL is added
Pyrrolidones (NMP) organic solvent, 140-160 DEG C of reaction 3-5h, obtained graphite dispersing solution is poured into Ultrasound Instrument, setting
Certain ultrasonic power, ultrasound are taken out after a certain period of time；
Step 2: graphene/carrier solution preparation
The poromerics carrier of 2500mg is added in graphite dispersing solution obtained in step 1, under the revolving speed of 2000r/min,
It is centrifuged 30min, takes upper liquid up to graphene/carrier solution, the graphene generated under high-speed rotation is wrapped in poromerics
Outside；
Step 3: graphene/support powder preparation
Graphene/carrier solution obtained in step 2 filters the NMP in removal graphene/carrier solution using cellulose membrane,
Cleaned three times with deionized water, then graphene/carrier granular be placed in the deionized water of 100mL, ultrasound obtain graphene/
Graphene/support powder is made by being freeze-dried in carrier aqueous solution.
Step 4: prepared by graphene polymer masterbatch
By the polyacrylate cream of graphene/support powder obtained in step 3 and the emulsifier of 0.7 parts by weight, 25 parts by weight
Liquid, dispersion and emulsion 0.5h, graphene/carrier are dispersed in polyacrylate dispersion in the form of protomere under high velocity agitation,
Obtain a kind of high concentration graphene polymer waterproof coating material masterbatch.
Specifically, the poromerics carrier select porous carbon, diatomite, zeolite powder, in aerosil extremely
Few one kind, poromerics diameter of carrier are less than 20um.
Specifically, the emulsifier is selected from 0P-10.
Specifically, the solid content of the polyacrylate dispersion is 25-35%.
Embodiment three
A kind of graphene polymer water-repellent paint masterbatch, graphene/carrier including 1 parts by weight, 0.9 parts by weight Emulsifier, 28
Parts by weight of polypropylene acid esters.
Preparation method are as follows:
Step 1: prepared by high concentration graphene solution
The high-purity natural crystalline flake graphite of 100mg80 mesh is weighed in 250mL polytetrafluoroethylene (PTFE) autoclave, the N methyl of 100mL is added
Pyrrolidones (NMP) organic solvent, 140-160 DEG C of reaction 3-5h, obtained graphite dispersing solution is poured into Ultrasound Instrument, setting
Certain ultrasonic power, ultrasound are taken out after a certain period of time；
Step 2: graphene/carrier solution preparation
The poromerics carrier of 2700mg is added in graphite dispersing solution obtained in step 1, under the revolving speed of 2000r/min,
It is centrifuged 30min, takes upper liquid up to graphene/carrier solution, the graphene generated under high-speed rotation is wrapped in poromerics
Outside；
Step 3: graphene/support powder preparation
Graphene/carrier solution obtained in step 2 filters the NMP in removal graphene/carrier solution using cellulose membrane,
Cleaned three times with deionized water, then graphene/carrier granular be placed in the deionized water of 100mL, ultrasound obtain graphene/
Graphene/support powder is made by being freeze-dried in carrier aqueous solution.
Step 4: prepared by graphene polymer masterbatch
By the polyacrylate cream of graphene/support powder obtained in step 3 and the emulsifier of 0.9 parts by weight, 28 parts by weight
Liquid, dispersion and emulsion 0.5h, graphene/carrier are dispersed in polyacrylate dispersion in the form of protomere under high velocity agitation,
Obtain a kind of high concentration graphene polymer waterproof coating material masterbatch.
Specifically, the poromerics carrier select porous carbon, diatomite, zeolite powder, in aerosil extremely
Few one kind, poromerics diameter of carrier are less than 20um.
Specifically, the emulsifier is selected from 0P-10.
Specifically, the solid content of the polyacrylate dispersion is 25-35%.
Example IV
A kind of graphene polymer water-repellent paint masterbatch, graphene/carrier including 1 parts by weight, 1 parts by weight Emulsifier, 30 weights
Measure part polyacrylate.
Preparation method are as follows:
Step 1: prepared by high concentration graphene solution
The high-purity natural crystalline flake graphite of 100mg80 mesh is weighed in 250mL polytetrafluoroethylene (PTFE) autoclave, the N methyl of 100mL is added
Pyrrolidones (NMP) organic solvent, 140-160 DEG C of reaction 3-5h, obtained graphite dispersing solution is poured into Ultrasound Instrument, setting
Certain ultrasonic power, ultrasound are taken out after a certain period of time；
Step 2: graphene/carrier solution preparation
The poromerics carrier of 3000mg is added in graphite dispersing solution obtained in step 1, under the revolving speed of 2000r/min,
It is centrifuged 30min, takes upper liquid up to graphene/carrier solution, the graphene generated under high-speed rotation is wrapped in poromerics
Outside；
Step 3: graphene/support powder preparation
Graphene/carrier solution obtained in step 2 filters the NMP in removal graphene/carrier solution using cellulose membrane,
Cleaned three times with deionized water, then graphene/carrier granular be placed in the deionized water of 100mL, ultrasound obtain graphene/
Graphene/support powder is made by being freeze-dried in carrier aqueous solution.
Step 4: prepared by graphene polymer masterbatch
By the polyacrylate cream of graphene/support powder obtained in step 3 and the emulsifier of 1 parts by weight, 30 parts by weight
Liquid, dispersion and emulsion 0.5h, graphene/carrier are dispersed in polyacrylate dispersion in the form of protomere under high velocity agitation,
Obtain a kind of high concentration graphene polymer waterproof coating material masterbatch.
Specifically, the poromerics carrier select porous carbon, diatomite, zeolite powder, in aerosil extremely
Few one kind, poromerics diameter of carrier are less than 20um.
Specifically, the emulsifier is selected from 0P-10.
Specifically, the solid content of the polyacrylate dispersion is 25-35%.
The present invention is not limited to the embodiment, anyone should learn that the structure made under the inspiration of the present invention becomes
Change, the technical schemes that are same or similar to the present invention are fallen within the scope of protection of the present invention.
Technology not described in detail in the present invention, shape, construction portion are well-known technique.
Claims (6)
1. a kind of graphene polymer water-repellent paint masterbatch, it is characterised in that: graphene/carrier including 1 parts by weight, 0.5-1
Parts by weight Emulsifier, 20-30 parts by weight of polypropylene acid esters.
2. a kind of graphene polymer water-repellent paint masterbatch according to claim 1, it is characterised in that: the graphene with
The mass ratio of carrier is 1:(20-30).
3. a kind of preparation method of graphene polymer water-repellent paint masterbatch, it is characterised in that: the following steps are included:
Step 1: prepared by high concentration graphene solution
The high-purity natural crystalline flake graphite of 100mg80 mesh is weighed in 250mL polytetrafluoroethylene (PTFE) autoclave, the N methyl of 100mL is added
Pyrrolidones (NMP) organic solvent, 140-160 DEG C of reaction 3-5h, obtained graphite dispersing solution is poured into Ultrasound Instrument, setting
Certain ultrasonic power, ultrasound are taken out after a certain period of time；
Step 2: graphene/carrier solution preparation
The poromerics carrier of 2000-3000mg is added in graphite dispersing solution obtained in step 1, in turning for 2000r/min
Under speed, it is centrifuged 30min, takes upper liquid up to graphene/carrier solution, the graphene generated under high-speed rotation is wrapped in micropore
Outside material；
Step 3: graphene/support powder preparation
Graphene/carrier solution obtained in step 2 filters the NMP in removal graphene/carrier solution using cellulose membrane,
Cleaned three times with deionized water, then graphene/carrier granular be placed in the deionized water of 100mL, ultrasound obtain graphene/
Graphene/support powder is made by being freeze-dried in carrier aqueous solution.
Step 4: prepared by graphene polymer masterbatch
By the polypropylene of graphene/support powder obtained in step 3 and the emulsifier of 0.5-1 parts by weight, 20-30 parts by weight
Acid esters lotion, dispersion and emulsion 0.5h, graphene/carrier are dispersed in polyacrylate cream in the form of protomere under high velocity agitation
In liquid, a kind of high concentration graphene polymer waterproof coating material masterbatch is obtained.
4. a kind of preparation method of graphene polymer water-repellent paint masterbatch according to claim 3, it is characterised in that: institute
It states poromerics carrier and selects at least one of porous carbon, diatomite, zeolite powder, aerosil, poromerics carries
Body partial size is less than 20um.
5. a kind of preparation method of graphene polymer water-repellent paint masterbatch according to claim 3, it is characterised in that: institute
It states emulsifier and is selected from one of 0P-10, AEO-9.
6. a kind of preparation method of graphene polymer water-repellent paint masterbatch according to claim 3, it is characterised in that: institute
The solid content for stating polyacrylate dispersion is 25-35%.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810263523.3A CN110157274A (en) | 2018-03-28 | 2018-03-28 | A kind of graphene polymer water-repellent paint masterbatch and preparation method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810263523.3A CN110157274A (en) | 2018-03-28 | 2018-03-28 | A kind of graphene polymer water-repellent paint masterbatch and preparation method |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103723708A (en) * | 2013-11-22 | 2014-04-16 | 盐城纳新天地新材料科技有限公司 | Preparation method of organic single-layer graphene solution |
| CN103738947A (en) * | 2013-11-22 | 2014-04-23 | 盐城纳新天地新材料科技有限公司 | Preparation method for single-layer graphene ethylene glycol solution |
| CN106987165A (en) * | 2017-05-26 | 2017-07-28 | 成都新柯力化工科技有限公司 | A kind of graphene polymer water-repellent paint masterbatch and preparation method |
| TWI607967B (en) * | 2017-01-04 | 2017-12-11 | 中原大學 | Method of producing graphene |
-
2018
- 2018-03-28 CN CN201810263523.3A patent/CN110157274A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103723708A (en) * | 2013-11-22 | 2014-04-16 | 盐城纳新天地新材料科技有限公司 | Preparation method of organic single-layer graphene solution |
| CN103738947A (en) * | 2013-11-22 | 2014-04-23 | 盐城纳新天地新材料科技有限公司 | Preparation method for single-layer graphene ethylene glycol solution |
| TWI607967B (en) * | 2017-01-04 | 2017-12-11 | 中原大學 | Method of producing graphene |
| CN106987165A (en) * | 2017-05-26 | 2017-07-28 | 成都新柯力化工科技有限公司 | A kind of graphene polymer water-repellent paint masterbatch and preparation method |
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Application publication date: 20190823 |