CN112625561A - Graphene dispersion liquid for modified polyester resin and preparation method thereof - Google Patents
Graphene dispersion liquid for modified polyester resin and preparation method thereof Download PDFInfo
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- CN112625561A CN112625561A CN202011575790.8A CN202011575790A CN112625561A CN 112625561 A CN112625561 A CN 112625561A CN 202011575790 A CN202011575790 A CN 202011575790A CN 112625561 A CN112625561 A CN 112625561A
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- graphene
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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
- C09D167/00—Coating compositions based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Coating compositions based on derivatives of such polymers
- C09D167/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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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
- C09D5/03—Powdery paints
- C09D5/033—Powdery paints characterised by the additives
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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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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
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Abstract
The invention relates to the technical field of polyester resin dispersion liquid, in particular to graphene dispersion liquid for modified polyester resin and a preparation method thereof. The graphene dispersion liquid for the modified polyester resin comprises the following components in percentage by mass: 1-20wt% of graphene; 80-99wt% of solvent; 0.01-1wt% of dispersing agent. Compared with the conventional graphene dispersion liquid, the graphene dispersion liquid for the modified polyester resin directly adopts the polyester resin synthetic raw material polyhydric alcohol and water as solvents, has high solid content, can realize the uniform dispersion of graphene in the polyester resin synthetic stage, and has the advantages that the coating of the cured coating of the polyester resin modified by the graphene dispersion liquid and the powder coating prepared by the polyester resin modified by the graphene dispersion liquid has high gloss, excellent mechanical property and weather resistance, and the corrosion resistance is obviously improved.
Description
Technical Field
The invention relates to the technical field of polyester resin dispersion liquid, in particular to graphene dispersion liquid for modified polyester resin and a preparation method thereof.
Background
Graphene (Graphene) is a two-dimensional carbon nanomaterial composed of carbon atoms in sp hybridized orbitals into a hexagonal honeycomb lattice. The graphene has excellent optical, electrical and mechanical properties, has important application prospects in the aspects of materials science, micro-nano processing, energy, biomedicine, drug delivery and the like, and is considered to be a revolutionary material in the future.
Chinese patents CN102585666A, CN104109450A-, CN105062304A, CN108300136A, CN106318155A, CN106867360A, CN106905822A, CN108641555A, CN108929624A, CN108976987A, CN110734689A and the like disclose a series of high-anticorrosion powder coatings containing graphene. Further, chinese patents CN106634474B, CN102964972B, CN106867360A, CN108300136A, CN201610671954.4, CN108929624B, etc. disclose a series of graphene-containing heat dissipating powder coatings. The principle is that graphene is added in the preparation process of the powder coating, and the heat dissipation performance of the powder coating is remarkably improved by utilizing the heat dissipation performance of the graphene. The application of the graphene in the powder coating has high requirements on the dispersion of the graphene in a resin matrix. However, in the prior art, graphene powder, resin and filler are mechanically mixed to produce the powder coating, and the graphene is difficult to uniformly disperse in the powder coating due to extrusion in the preparation process of the powder coating, so that the performances of the powder coating are unevenly distributed.
Disclosure of Invention
In order to overcome the defect of poor dispersion effect of the existing graphene, the invention provides a graphene dispersion liquid for modified polyester resin and a preparation method thereof.
The technical scheme adopted by the invention for solving the technical problems is as follows: the graphene dispersion liquid for the modified polyester resin comprises the following components in percentage by mass: 1-20wt% of graphene; 80-99wt% of solvent; 0.01-1wt% of dispersing agent.
According to another embodiment of the present invention, further comprising that the graphene is a mixture of one or more of single-layer graphene, multi-layer graphene, graphene oxide or modified graphene.
According to another embodiment of the present invention, further comprising the solvent is a mixture of one or more of distilled water, neopentyl glycol (NPG), Ethylene Glycol (EG), methyl propylene glycol (MPDI), ethyl butyl propylene glycol (BEPD) or Cyclohexanedimethanol (CHDM).
According to another embodiment of the present invention, the solvent is a mixture of any one of neopentyl glycol (NPG), Ethylene Glycol (EG), methyl propylene glycol (MPDI), ethyl butyl propylene glycol (BEPD) or cyclohexane dimethanol (CHDM) and distilled water, wherein the distilled water accounts for 1-30 wt% of the total solvent.
According to another embodiment of the present invention, the dispersant is one or more of an anionic surfactant, a cationic surfactant or a mixture of nonionic surfactants.
According to another embodiment of the present invention, further comprising, the nonionic surfactant is selected from one or more of polyvinyl alcohol, polyvinyl formal, hydroxymethyl cellulose, polyvinylpyrrolidone, N-methylpyrrolidone, 1, 3-dimethyl-2-imidazolidinone dimethylformamide, dimethylacetamide, dimethyl sulfoxide, polyethylene glycol octyl phenyl ether, polyalkoxyethyl ether ester and polyoxyethylene (20) -sorbitan monooleate.
According to another embodiment of the present invention, further comprising, the anionic surfactant is selected from one or a mixture of two of sodium dodecyl sulfate and sodium dodecyl benzene sulfonate.
According to another embodiment of the present invention, further comprising, the cationic surfactant is selected from one or more of cetyl trimethyl ammonium bromide, polyallylamine hydrochloride, polyacrylamide.
A preparation method of graphene dispersion liquid for modified polyester resin comprises the following steps:
1) weighing graphene and a dispersing agent according to the formula ratio, adding a solvent into a dispersion tank at a mass ratio of 10-15:1, adjusting the rotating speed of a shearing dispersion machine to 800-plus-one 1000rpm, adding the dispersing agent into the dispersion tank until the dispersing agent is dissolved, then adding the graphene, stirring and uniformly dispersing, adjusting the rotating speed of the dispersion machine to 1200-plus-one 2000rpm, and dispersing for 1-3 hours to obtain a suspension of the graphene;
2) transferring the graphene suspension into an ultrasonic container for ultrasonic treatment, wherein the ultrasonic frequency is 19-21kHz, and the ultrasonic time is 10-30 min;
3) centrifuging the graphene suspension subjected to ultrasonic treatment, removing supernatant, taking a lower-layer slurry-like substance (3-10 layers of graphene which are stripped and dispersed, and the solid content is 30-90 wt.%), mixing the lower-layer slurry-like substance with a solvent which is 10-15 times the mass of the lower-layer slurry-like substance, performing ultrasonic treatment, repeating the step for 2-3 times, performing solid content calibration on the slurry-like substance (3-10 layers of graphene which are fully stripped and dispersed, and the solid content is 40-80wt.%) obtained after centrifugal treatment, and adding the solvent and the dispersing agent to ensure that the components of the mixture are respectively in mass percent: 1-20wt% of graphene, 80-99wt% of solvent and 0.01-1wt% of dispersant, stirring and mixing for 10-20min, and uniformly dispersing to obtain the graphene dispersion liquid with given concentration.
The graphene dispersion liquid for the modified polyester resin has the beneficial effects that compared with the conventional graphene dispersion liquid, the graphene dispersion liquid directly adopts polyester resin synthetic raw material polyhydric alcohol and water as solvents, the solid content is high, the uniform dispersion of graphene can be realized in the polyester resin synthetic stage, and the coating of the polyester resin modified by the graphene dispersion liquid and the powder coating prepared by the polyester resin modified by the graphene dispersion liquid has high gloss, excellent mechanical property and weather resistance and is remarkably improved in corrosion resistance.
Detailed Description
The graphene dispersion liquid for the modified polyester resin comprises the following components in percentage by mass: 1-20wt% of graphene; 80-99wt% of solvent; 0.01-1wt% of dispersing agent.
According to another embodiment of the present invention, further comprising that the graphene is a mixture of one or more of single-layer graphene, multi-layer graphene, graphene oxide or modified graphene.
According to another embodiment of the present invention, further comprising the solvent is a mixture of one or more of distilled water, neopentyl glycol (NPG), Ethylene Glycol (EG), methyl propylene glycol (MPDI), ethyl butyl propylene glycol (BEPD) or Cyclohexanedimethanol (CHDM).
According to another embodiment of the present invention, the solvent is a mixture of any one of neopentyl glycol (NPG), Ethylene Glycol (EG), methyl propylene glycol (MPDI), ethyl butyl propylene glycol (BEPD) or cyclohexane dimethanol (CHDM) and distilled water, wherein the distilled water accounts for 1-30 wt% of the total solvent.
According to another embodiment of the present invention, the dispersant is one or more of an anionic surfactant, a cationic surfactant or a mixture of nonionic surfactants.
According to another embodiment of the present invention, further comprising, the nonionic surfactant is selected from one or more of polyvinyl alcohol, polyvinyl formal, hydroxymethyl cellulose, polyvinylpyrrolidone, N-methylpyrrolidone, 1, 3-dimethyl-2-imidazolidinone dimethylformamide, dimethylacetamide, dimethyl sulfoxide, polyethylene glycol octyl phenyl ether, polyalkoxyethyl ether ester and polyoxyethylene (20) -sorbitan monooleate.
According to another embodiment of the present invention, further comprising, the anionic surfactant is selected from one or a mixture of two of sodium dodecyl sulfate and sodium dodecyl benzene sulfonate.
According to another embodiment of the present invention, further comprising, the cationic surfactant is selected from one or more of cetyl trimethyl ammonium bromide, polyallylamine hydrochloride, polyacrylamide.
A preparation method of graphene dispersion liquid for modified polyester resin comprises the following steps:
1) weighing graphene and a dispersing agent according to the formula ratio, adding a solvent into a dispersion tank at a mass ratio of 10-15:1, adjusting the rotating speed of a shearing dispersion machine to 800-plus-one 1000rpm, adding the dispersing agent into the dispersion tank until the dispersing agent is dissolved, then adding the graphene, stirring and uniformly dispersing, adjusting the rotating speed of the dispersion machine to 1200-plus-one 2000rpm, and dispersing for 1-3 hours to obtain a suspension of the graphene;
2) transferring the graphene suspension into an ultrasonic container for ultrasonic treatment, wherein the ultrasonic frequency is 19-21kHz, and the ultrasonic time is 10-30 min;
the purpose of ultrasonic treatment is to open graphene sheet layers and refine graphene sheet diameters, so that graphene is fully dispersed in a solvent.
3) Centrifuging the graphene suspension subjected to ultrasonic treatment, removing supernatant, taking a lower-layer slurry-like substance (3-10 layers of graphene which are stripped and dispersed, and the solid content is 30-90 wt.%), mixing the lower-layer slurry-like substance with a solvent which is 10-15 times the mass of the lower-layer slurry-like substance, performing ultrasonic treatment, repeating the step for 2-3 times, performing solid content calibration on the slurry-like substance (3-10 layers of graphene which are fully stripped and dispersed, and the solid content is 40-80wt.%) obtained after centrifugal treatment, and adding the solvent and the dispersing agent to ensure that the components of the mixture are respectively in mass percent: 1-20wt% of graphene, 80-99wt% of solvent and 0.01-1wt% of dispersant, stirring and mixing for 10-20min, and uniformly dispersing to obtain the graphene dispersion liquid with given concentration.
The first embodiment is as follows:
preparation of a neopentyl glycol dispersion containing 10wt% graphene:
adding a proper amount of 1000g of solvent (a neopentyl glycol mixed system containing 20% of water) into a dispersion tank, adjusting the rotating speed of a high-speed shearing dispersion machine to 800-1000rpm, putting a dispersing agent (1g of polyvinylpyrrolidone) into the dispersion tank until the dispersing agent is dissolved, then adding 100g of commercialized graphene, stirring and uniformly dispersing, adjusting the rotating speed of the dispersion machine to 1200-2000rpm, and adjusting the dispersion time to 1-3 hours to obtain the graphene suspension. 2) And transferring the graphene suspension into an ultrasonic container for ultrasonic treatment, wherein the ultrasonic frequency is 19-21kHz, and the ultrasonic time is 10-30 min. 3) Centrifuging the graphene suspension subjected to ultrasonic treatment, removing supernatant, taking the lower layer slurry-like substance, mixing with a proper amount of solvent, and performing ultrasonic treatment. Repeating the step for 2-3 times, mixing 170g of slurry-like substance (containing 55 wt% of graphene) obtained after ultrasonic treatment with 765g of neopentyl glycol serving as a solvent according to the formula, adding a dispersing agent according to the formula, and stirring and mixing uniformly to obtain the 10wt% neopentyl glycol graphene dispersion liquid.
The performance of the graphene dispersion can be reflected by the performance of the synthesized polyester resin and the powder coating.
Preparation of graphene-containing polyester resin
In Table 1, A to F are the primary properties of examples of the present invention and their corresponding polyester resins.
The preparation method comprises the following steps: putting the polyol, the branching agent, the graphene dispersion liquid, the aromatic acid and a proper amount of catalyst into a 5-liter glass reaction kettle at the same time, slowly heating to 235-255 ℃ in a nitrogen atmosphere and maintaining, sampling and detecting that the Acid Value (AV) reaches 5-15 (unit mgKOH/g resin, the same applies below) after the system is clarified, adding secondary acidolysis agents IPA, ADA, CHDA/FCC and TMA and the like and maintaining the temperature at 235-250 ℃ for acidolysis and end capping. After the acid value of the polyester reaches a set value, cooling to 230-240 ℃ and carrying out vacuum polycondensation for a period of time to enable the acid value and the hydroxyl value of the polyester to reach a set range; and finally, cooling to 180-230 ℃, adding an antioxidant and a curing accelerator, maintaining for 5-30 min, and discharging. Wherein the acid value control indexes at different stages are also shown in Table 1.
Table 1, formulation of polyester resin for highly anticorrosive powder coating, control of acid value during production and performance index of final resin. The following table units: and (4) parts by mass.
The saturated polyester resins a to G synthesized in the examples were weighed and mixed with a curing agent (triglycidyl isocyanurate (TGIC), blocked isocyanate (B1530)), a leveling agent, benzoin, 701B, titanium dioxide, barium sulfate, etc. according to the proportions in table 2, and melted by a screw extruder, extruded, tabletted, crushed, and sieved, respectively, to prepare a powder coating. The powder coating was then sprayed on the iron plate after surface phosphating, various properties of the system were tested after curing under appropriate curing conditions, and various properties of the coating were then tested, with the results as follows.
Table 2 composition of the powder coating and coating properties. The following table units: and (4) parts by mass.
As can be seen from Table 2, the coating layer of the polyester resin of the present invention after being cured by the powder coating has the characteristics of high gloss and excellent mechanical properties. Compared with the conventional polyester resin without added graphene, the introduction of the graphene can obviously improve the weather resistance and the corrosion resistance. Considering that the anti-corrosion performance of the powder coating specified by the national standard requires that the unilateral corrosion width of 500h is not more than 2mm, the unilateral corrosion width of 1000h is not more than 4 mm. From table 2, it can be seen that the corrosion resistance of the polyester resin of the present invention is significantly improved, even the corrosion resistance exceeds 1000 h.
The foregoing description is intended to be illustrative rather than limiting, and it will be appreciated by those skilled in the art that many modifications, variations or equivalents may be made without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (9)
1. The graphene dispersion liquid for the modified polyester resin is characterized by comprising the following components in percentage by mass: 1-20wt% of graphene; 80-99wt% of solvent; 0.01-1wt% of dispersing agent.
2. The graphene dispersion liquid for a modified polyester resin according to claim 1, wherein the graphene is one or a mixture of single-layer graphene, multi-layer graphene, graphene oxide, or modified graphene.
3. The graphene dispersion liquid for modified polyester resin according to claim 1, wherein the solvent is one or more selected from distilled water, neopentyl glycol (NPG), Ethylene Glycol (EG), methyl propylene glycol (MPDI), ethyl butyl propylene glycol (BEPD) and cyclohexane dimethanol (CHDM).
4. The graphene dispersion liquid for modified polyester resin according to claim 3, wherein the solvent is a mixture of distilled water and at least one of neopentyl glycol (NPG), Ethylene Glycol (EG), methyl propylene glycol (MPDI), ethyl butyl propylene glycol (BEPD) or cyclohexane dimethanol (CHDM), and the distilled water accounts for 1-30 wt% of the total solvent amount.
5. The graphene dispersion liquid for modified polyester resins according to claim 1, wherein the dispersant is one or more selected from an anionic surfactant, a cationic surfactant and a nonionic surfactant.
6. The graphene dispersion liquid for modified polyester resins according to claim 5, wherein the nonionic surfactant is one or more selected from the group consisting of polyvinyl alcohol, polyvinyl formal, hydroxymethyl cellulose, polyvinyl pyrrolidone, N-methyl pyrrolidone, 1, 3-dimethyl-2-imidazolidinone dimethylformamide, dimethylacetamide, dimethyl sulfoxide, polyethylene glycol octylphenyl ether, polyalkoxyethyl ether ester and polyoxyethylene (20) -sorbitan monooleate.
7. The graphene dispersion liquid for modified polyester resins according to claim 5, wherein the anionic surfactant is one or a mixture of two selected from sodium dodecyl sulfate and sodium dodecyl benzene sulfonate.
8. The graphene dispersion liquid for modified polyester resin according to claim 5, wherein the cationic surfactant is one or more selected from the group consisting of cetyltrimethylammonium bromide, polyallylamine hydrochloride, and polyacrylamide.
9. A method for preparing the graphene dispersion liquid for modified polyester resin according to claims 1 to 8, comprising the steps of:
1) weighing graphene and a dispersing agent according to the formula ratio, adding a solvent into a dispersion tank at a mass ratio of 10-15:1, adjusting the rotating speed of a shearing dispersion machine to 800-plus-one 1000rpm, adding the dispersing agent into the dispersion tank until the dispersing agent is dissolved, then adding the graphene, stirring and uniformly dispersing, adjusting the rotating speed of the dispersion machine to 1200-plus-one 2000rpm, and dispersing for 1-3 hours to obtain a suspension of the graphene;
2) transferring the graphene suspension into an ultrasonic container for ultrasonic treatment, wherein the ultrasonic frequency is 19-21kHz, and the ultrasonic time is 10-30 min;
3) centrifuging the graphene suspension subjected to ultrasonic treatment, removing supernatant, taking a lower-layer slurry-like substance (3-10 layers of graphene which are stripped and dispersed, and the solid content is 30-90 wt.%), mixing the lower-layer slurry-like substance with a solvent which is 10-15 times the mass of the lower-layer slurry-like substance, performing ultrasonic treatment, repeating the step for 2-3 times, performing solid content calibration on the slurry-like substance (3-10 layers of graphene which are fully stripped and dispersed, and the solid content is 40-80wt.%) obtained after centrifugal treatment, and adding the solvent and the dispersing agent to ensure that the components of the mixture are respectively in mass percent: 1-20wt% of graphene, 80-99wt% of solvent and 0.01-1wt% of dispersant, stirring and mixing for 10-20min, and uniformly dispersing to obtain the graphene dispersion liquid with given concentration.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114106670A (en) * | 2021-12-23 | 2022-03-01 | 安徽神剑新材料股份有限公司 | Electromagnetic shielding powder coating and preparation method thereof |
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| CN110511367A (en) * | 2019-08-20 | 2019-11-29 | 安徽神剑新材料股份有限公司 | A kind of polyester resin for powder coating of containing graphene |
| CN111303676A (en) * | 2020-03-09 | 2020-06-19 | 北京石墨烯研究院 | Graphene dispersion liquid, preparation method thereof and anticorrosive paint applying graphene dispersion liquid |
| CN111518459A (en) * | 2020-06-22 | 2020-08-11 | 北京石墨烯研究院 | Water-based graphene light anticorrosive paint and preparation method thereof |
| CN111592640A (en) * | 2020-05-12 | 2020-08-28 | 浙江恒澜科技有限公司 | Preparation method of graphene modified polyester composite material based on liquid phase stripping |
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- 2020-12-28 CN CN202011575790.8A patent/CN112625561A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110511367A (en) * | 2019-08-20 | 2019-11-29 | 安徽神剑新材料股份有限公司 | A kind of polyester resin for powder coating of containing graphene |
| CN111303676A (en) * | 2020-03-09 | 2020-06-19 | 北京石墨烯研究院 | Graphene dispersion liquid, preparation method thereof and anticorrosive paint applying graphene dispersion liquid |
| CN111592640A (en) * | 2020-05-12 | 2020-08-28 | 浙江恒澜科技有限公司 | Preparation method of graphene modified polyester composite material based on liquid phase stripping |
| CN111518459A (en) * | 2020-06-22 | 2020-08-11 | 北京石墨烯研究院 | Water-based graphene light anticorrosive paint and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114106670A (en) * | 2021-12-23 | 2022-03-01 | 安徽神剑新材料股份有限公司 | Electromagnetic shielding powder coating and preparation method thereof |
| CN114106670B (en) * | 2021-12-23 | 2022-08-05 | 安徽神剑新材料股份有限公司 | Electromagnetic shielding powder coating and preparation method thereof |
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