CN115678398A - Antistatic waterborne polyurethane coating material and preparation method thereof - Google Patents
Antistatic waterborne polyurethane coating material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an antistatic waterborne polyurethane coating material and a preparation method thereof. The antistatic aqueous polyurethane coating material is prepared from raw materials including an aqueous polyurethane solution, a water-dispersible inorganic nano filler and a water-dispersible conductive organic filler, wherein the mass ratio of the aqueous polyurethane to the water-dispersible inorganic nano filler to the water-dispersible conductive organic filler is 100:0.1 to 5:0.1 to 5; and uniformly mixing the raw materials according to the proportion, defoaming and drying to obtain the antistatic waterborne polyurethane coating material. The antistatic waterborne polyurethane coating material has the advantages of good mechanical property, high strength and good antistatic property.
Description
Technical Field
The invention relates to the field of preparation of polymer composite materials, in particular to an antistatic waterborne polyurethane coating material and a preparation method thereof.
Background
The waterborne polyurethane takes water as a dispersing medium instead of an organic solvent, has the characteristics of low toxicity, safety, reliability, almost no pollution and the like, is nontoxic and tasteless, and accords with the green and sustainable development policy. The formation process of the water-based polyurethane is a dispersed emulsion in which the polyurethane is uniformly dispersed in water under the action of high-speed shearing. Compared with solvent type polyurethane, the waterborne polyurethane has the following characteristics: (1) Water is used as a dispersion medium, is colorless, tasteless and nontoxic, and is green and environment-friendly compared with solvent type polyurethane. (2) The emulsifier is introduced into the reaction system to prepare the self-emulsifying aqueous polyurethane, so that the aqueous polyurethane can be emulsified to form stable emulsion, and the emulsifier participating in the reaction can also be regarded as a chain extender with hydrophilic groups. (3) In consideration of the nature of the active groups on the waterborne polyurethane, the waterborne polyurethane can be modified by other resins or inorganic fillers, so that the cost can be reduced and the performance can be improved to a certain extent.
The composite material prepared by adding the nano inorganic filler into the high molecular polymer matrix is one of important methods for improving the comprehensive performance of the high molecular material. The nano material has the structural characteristics of large specific surface area, smaller particle spacing, higher surface energy and the like, has the characteristics of chemical activity, excellent mechanical property and the like, and can obviously improve the mechanical property of the composite material when being applied to high molecular polymers. The filler particles can be classified into zero-dimensional nanomaterials (zinc oxide, silicon dioxide, etc.), one-dimensional nanomaterials (fibers, carbon nanotubes, etc.), and two-dimensional nanomaterials (montmorillonite, graphene, etc.) according to the shape of the filler particles. The filler particles are added not only for the purpose of improving the material properties but also for cost saving.
Polyurethane can be used for preparing antistatic materials, but the mechanical property of the waterborne polyurethane material is poor, the tensile strength and the elongation at break are not ideal, and the tensile strength of the antistatic polyurethane material in the prior art is limited in practical application, so that the waterborne polyurethane is rarely adopted as a raw material, and the antistatic effect is also needed to be improved.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides an antistatic waterborne polyurethane coating material and a preparation method thereof.
Aiming at the defect of poor mechanical property of the waterborne polyurethane, the invention provides a modification method for improving the mechanical property of the waterborne polyurethane by using an inorganic filler, so that the coating material has higher tensile strength; meanwhile, poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid (PEDOT: PSS) is adopted to modify the waterborne polyurethane, so that the waterborne polyurethane has better antistatic property.
The invention aims to provide an antistatic waterborne polyurethane coating material.
The antistatic water-based polyurethane coating material is prepared from raw materials including a water-based polyurethane solution, a water-dispersible inorganic nano filler and a water-dispersible conductive organic filler;
the mass ratio of the water-based polyurethane to the water-dispersible inorganic nano filler to the water-dispersible conductive organic filler is 100:0.1 to 5:0.1 to 5; the mass ratio is preferably 100:0.1 to 0.5:0.1 to 0.5; the aqueous polyurethane refers to the mass of the aqueous polyurethane excluding water in the aqueous polyurethane solution, and the water-dispersible inorganic nano filler and the water-dispersible conductive organic filler, if the aqueous polyurethane solution is a solution, refer to the mass excluding a solvent in the solution.
The water-dispersible inorganic nano-filler can improve the mechanical property of the aqueous polyurethane coating, and the water-dispersible conductive organic filler can also play a role in improving the mechanical property besides improving the conductivity.
In a preferred embodiment of the present invention,
the aqueous polyurethane solution is a cationic aqueous polyurethane solution or an anionic aqueous polyurethane solution.
In a preferred embodiment of the present invention,
the solid content of the aqueous polyurethane solution is 10-25%;
the aqueous polyurethane solution has high solid content, which can easily cause agglomeration and is not easy to disperse, and has low solid content which is difficult to form a film, so that a proper solid content range needs to be selected.
In a preferred embodiment of the present invention,
the total water content of the mixed solution of the aqueous polyurethane solution, the water dispersible inorganic nano filler and the water dispersible conductive organic filler is 70-90 percent, and the total water content is preferably 80-85 percent;
too low a total water content can result in uneven filler dispersion, while too high a total water content can reduce the performance of the coating material.
In a preferred embodiment of the present invention,
the water-dispersible inorganic nano filler is at least one of graphene oxide, hydroxyl modified two-dimensional inorganic nano filler and carboxyl modified two-dimensional inorganic nano filler.
In a preferred embodiment of the present invention,
the hydroxyl modified two-dimensional inorganic nano filler is preferably boron nitride; and/or the presence of a gas in the atmosphere,
the carboxyl modified two-dimensional inorganic nano-filler is preferably silica nanospheres.
In a preferred embodiment of the present invention,
the water-dispersible conductive filler is poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid (PEDOT: PSS); the common water-dispersible conductive filler can be carbon black, carbon nano-tube, montmorillonite and the like, and can be used as the water-dispersible conductive filler of the invention.
The invention also aims to provide a preparation method of the antistatic waterborne polyurethane coating material, which comprises the following steps:
the antistatic waterborne polyurethane coating material is prepared by uniformly mixing the raw materials according to the proportion, defoaming and drying.
The method comprises the following specific steps:
1. proportionally adding a water-dispersible inorganic nano filler and a water-dispersible conductive organic filler into an aqueous polyurethane solution for mixing, and performing ultrasonic and high-speed stirring to obtain a solution with uniformly dispersed fillers;
2. defoaming the blended solution in the step 1, and pouring the defoamed solution into a mold;
3. drying in a blower oven to obtain the film.
In a preferred embodiment of the present invention,
the mixing temperature is 20-60 ℃, and the mixture is stirred at high speed at the temperature;
the drying temperature is 45-100 ℃, and the temperature set by the oven is in the temperature range.
Compared with the prior art, the invention has the beneficial effects that:
the antistatic waterborne polyurethane coating material is prepared by taking waterborne polyurethane as a main raw material, and the mechanical property of the waterborne polyurethane is improved through the water-dispersible inorganic nano-filler, so that the coating material has higher strength; meanwhile, poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid (PEDOT: PSS) is adopted to modify the waterborne polyurethane, so that the waterborne polyurethane has better antistatic property and the conductivity is improved by one order of magnitude.
The antistatic waterborne polyurethane coating material prepared by the invention has good mechanical property and higher tensile strength which reaches more than 20MPa, and the application range in practical use is greatly enlarged.
Drawings
FIG. 1 is a stress-strain graph of examples 1 to 5 and comparative examples 1 to 3.
Detailed Description
While the present invention will be described in detail and with reference to the specific embodiments thereof, it should be understood that the following detailed description is only for illustrative purposes and is not intended to limit the scope of the present invention, as those skilled in the art will appreciate numerous insubstantial modifications and variations therefrom.
The raw materials used in the examples and the comparative examples are all conventional commercial raw materials;
the specifications of the main raw materials are shown in table 1;
TABLE 1 Main raw material specification and manufacturer
The tensile and fracture test reference standard GB-T508-2009;
according to the test mode of national standard GB-T508-2009, cutting the sample into dumbbell-shaped sample strips with the thickness of 0.5mm-1mm, the width of the test area of 4mm and the length of 15mm, and testing at the speed of 500 mm.min -1 The tensile rate of (2) was tested.
Conductivity test method:
at room temperature, usingTesting the conductivity of the film by a Concept 50 model broadband dielectric impedance spectrometer of Novocontrol in Germany; test frequency of 10 -1 Hz-10 7 Hz, the testing temperature is room temperature, the sample size is a film with the diameter of 20-25mm and the thickness of 0.5-1 mm;
example 1
Preparing a solution according to the mass ratio of the waterborne polyurethane to the graphene oxide to the PEDOT to PSS of 100. The graphene oxide is prepared by diluting a graphene oxide stock solution, adding deionized water to dilute the graphene oxide stock solution to 0.3wt%, and stirring the diluted solution at normal temperature for 6 hours to prepare a graphene oxide aqueous solution with the mass concentration of 0.3 wt%; the water-based polyurethane is a cationic water-based polyurethane solution, and the solid content of the water-based polyurethane is 19 percent; the total water content of the mixed solution of the waterborne polyurethane, the graphene oxide and the PEDOT PSS is 80 percent;
placing the mixed solution into a 500ml three-neck flask, keeping the mixing temperature at normal temperature, ultrasonically stirring at normal temperature for 4h, standing the mixed solution for one night for defoaming, pouring the mixed solution into a polytetrafluoroethylene mold with the thickness of 10cm multiplied by 3mm, standing at room temperature, and evaporating water in the solution. And (3) putting the film into a blast oven, drying for 10h at the temperature of 60 ℃, taking out, tearing the film from the sample to obtain the film with the length and width of 10cm multiplied by 10cm, and thus obtaining the antistatic waterborne polyurethane coating material.
Example 2
Preparing a solution according to the mass ratio of the waterborne polyurethane to the graphene oxide to the PEDOT to PSS of 100. The graphene oxide is prepared by diluting a graphene oxide stock solution, adding deionized water to dilute the graphene oxide stock solution to 0.3wt%, and stirring the diluted solution at normal temperature for 6 hours to prepare a graphene oxide aqueous solution with the mass concentration of 0.3 wt%; the water-based polyurethane is a cationic water-based polyurethane solution, and the solid content of the water-based polyurethane is 19 percent; the total water content of the mixed solution of the waterborne polyurethane, the graphene oxide and the PEDOT PSS is 80 percent;
placing the mixed solution into a 500ml three-neck flask, keeping the mixing temperature at normal temperature, ultrasonically stirring for 4h at normal temperature, standing the mixed solution overnight for defoaming, pouring the mixed solution into a polytetrafluoroethylene mould with the thickness of 10cm multiplied by 3mm, standing at room temperature, and evaporating water in the solution. And (3) putting the film into a blast oven, drying for 10h at the temperature of 60 ℃, taking out, tearing the film from the sample to obtain the film with the length and width of 10cm multiplied by 10cm, and thus obtaining the antistatic waterborne polyurethane coating material.
Example 3
Preparing a solution according to the mass ratio of the waterborne polyurethane to the graphene oxide to the PEDOT to the PSS of 100. The graphene oxide is prepared by diluting a graphene oxide stock solution, adding deionized water to dilute the graphene oxide stock solution to 0.3wt%, and stirring the diluted solution at normal temperature for 6 hours to prepare a graphene oxide aqueous solution with the mass concentration of 0.3 wt%; the water-based polyurethane is a cationic water-based polyurethane solution, and the solid content of the water-based polyurethane solution is 19 percent; the total water content of the mixed solution of the waterborne polyurethane, the graphene oxide and the PEDOT PSS is 80 percent;
placing the mixed solution into a 500ml three-neck flask, keeping the mixing temperature at normal temperature, ultrasonically stirring at normal temperature for 4h, standing the mixed solution for one night for defoaming, pouring the mixed solution into a polytetrafluoroethylene mold with the thickness of 10cm multiplied by 3mm, standing at room temperature, and evaporating water in the solution. And (3) putting the film into a blast oven, drying for 10h at the temperature of 60 ℃, taking out, tearing the film from the sample to obtain the film with the length and width of 10cm multiplied by 10cm, and thus obtaining the antistatic waterborne polyurethane coating material.
Example 4
Preparing a solution according to the mass ratio of the waterborne polyurethane to the graphene oxide to the PEDOT to the PSS of 100:0.1, wherein the mass ratio of the raw materials excluding the solvent is as follows. The graphene oxide is prepared by diluting a graphene oxide stock solution, adding deionized water to dilute the graphene oxide stock solution to 0.3wt%, and stirring the diluted solution at normal temperature for 6 hours to prepare a graphene oxide aqueous solution with the mass concentration of 0.3 wt%; the aqueous polyurethane is an anionic aqueous polyurethane solution, and the solid content of the aqueous polyurethane solution is 19 percent; the total water content of the mixed solution of the waterborne polyurethane, the graphene oxide and the PEDOT PSS is 80 percent;
placing the mixed solution into a 500ml three-neck flask, keeping the mixing temperature at normal temperature, ultrasonically stirring at normal temperature for 4h, standing the mixed solution for one night for defoaming, pouring the mixed solution into a polytetrafluoroethylene mold with the thickness of 10cm multiplied by 3mm, standing at room temperature, and evaporating water in the solution. And (3) putting the film into a blast oven, drying for 10h at the temperature of 60 ℃, taking out, tearing the film from the sample to obtain the film with the length and width of 10cm multiplied by 10cm, and thus obtaining the antistatic waterborne polyurethane coating material.
Example 5
Preparing a solution according to the mass ratio of the waterborne polyurethane to the graphene oxide to the PEDOT to the PSS of 100: 0.1. The graphene oxide is prepared by diluting a graphene oxide stock solution, adding deionized water to dilute the graphene oxide stock solution to 0.3wt%, and stirring the diluted solution at normal temperature for 6 hours to prepare a graphene oxide aqueous solution with the mass concentration of 0.3 wt%; the water-based polyurethane is a cationic water-based polyurethane solution, and the solid content of the water-based polyurethane is 25 percent; the total water content of the mixed solution of the waterborne polyurethane, the graphene oxide and the PEDOT PSS is 85 percent;
placing the mixed solution into a 500ml three-neck flask, keeping the mixing temperature at 60 ℃, ultrasonically stirring for 4h at normal temperature, standing the mixed solution overnight for defoaming, pouring the mixed solution into a polytetrafluoroethylene mold with the thickness of 10cm multiplied by 3mm, standing at room temperature, and evaporating water in the solution. And (3) putting the film into a blast oven, drying for 10h at 100 ℃, taking out, tearing the film from the sample to obtain a film with the length and width of 10cm multiplied by 10cm, and thus obtaining the antistatic waterborne polyurethane coating material.
Comparative example 1
Comparative example 1 is a cationic aqueous polyurethane solution, the solid content is 19%, the aqueous polyurethane solution is poured into a mold, placed in an oven after standing overnight, and the water in the sample is dried at 60 ℃ to obtain a colorless and transparent film without any filler.
Comparative example 2
In contrast to example 1, no graphene oxide was added.
According to the mass ratio of waterborne polyurethane to PEDOT to PSS of 100:0.1 preparation solution means the mass ratio of each raw material excluding the solvent. The water-based polyurethane is a cationic water-based polyurethane solution, and the solid content of the water-based polyurethane is 19 percent; the total water content of the obtained mixed solution of waterborne polyurethane and PEDOT and PSS is 80 percent;
placing the mixed solution into a 500ml three-neck flask, keeping the mixing temperature at normal temperature, ultrasonically stirring at normal temperature for 4h, standing the mixed solution for one night for defoaming, pouring the mixed solution into a polytetrafluoroethylene mold with the thickness of 10cm multiplied by 3mm, standing at room temperature, and evaporating water in the solution. And (3) putting the film into a blast oven, drying for 10 hours at the temperature of 60 ℃, taking out the film, tearing the film from the sample to obtain the film with the length and width of 10cm multiplied by 10cm, and thus obtaining the antistatic waterborne polyurethane coating material.
Comparative example 3
In contrast to example 1, no PEDOT: PSS was added.
Preparing a solution according to the mass ratio of the aqueous polyurethane to the graphene oxide of 100.1, wherein the mass ratio refers to the mass ratio of the raw materials excluding the solvent. The graphene oxide is prepared by diluting a graphene oxide stock solution, adding deionized water to dilute the graphene oxide stock solution to 0.3wt%, and stirring the diluted solution at normal temperature for 6 hours to prepare a graphene oxide aqueous solution with the mass concentration of 0.3 wt%; the water-based polyurethane is a cationic water-based polyurethane solution, and the solid content of the water-based polyurethane is 19 percent; the total water content of the obtained mixed solution of the waterborne polyurethane and the graphene oxide is 80 percent;
placing the mixed solution into a 500ml three-neck flask, keeping the mixing temperature at normal temperature, ultrasonically stirring at normal temperature for 4h, standing the mixed solution for one night for defoaming, pouring the mixed solution into a polytetrafluoroethylene mold with the thickness of 10cm multiplied by 3mm, standing at room temperature, and evaporating water in the solution. And (3) putting the film into a blast oven, drying for 10 hours at the temperature of 60 ℃, taking out the film, tearing the film from the sample to obtain the film with the length and width of 10cm multiplied by 10cm, and thus obtaining the antistatic waterborne polyurethane coating material.
FIG. 1 is a stress-strain curve diagram of examples 1-5 and comparative examples 1-3, and it can be seen from FIG. 1 that the mechanical properties of the waterborne polyurethane are greatly improved after the filler is added, and simultaneously, after the graphene oxide and PEDOT are added, the tensile strength and elongation at break of the sample are remarkably improved, and the two fillers have a coordination effect on the improvement of the mechanical properties of the waterborne polyurethane.
TABLE 2 mechanical Property test results of examples 1 to 5 and comparative examples 1 to 3
| Sample (I) | Tensile strength (Mpa) | Elongation at Break (%) |
| Example 1 | 19.8±4.0 | 637±62 |
| Example 2 | 25.9±2.1 | 601±52 |
| Example 3 | 38.6±3.9 | 558±25 |
| Example 4 | 21.4±3.4 | 530±26 |
| Example 5 | 23.1±4.9 | 555±46 |
| Comparative example 1 | 5.9±1.1 | 428±29 |
| Comparative example 2 | 13.5±2.7 | 525±33 |
| Comparative example 3 | 13.8±5.1 | 499±65 |
As shown in Table 3, after the filler is added, the conductivity of the waterborne polyurethane composite material is increased, the conductivity is enhanced, and the resistivity is reduced, but from the table, after the PEDOT, PSS and graphene oxide are added, the conductivity is increased more obviously, and is increased by one order of magnitude, so that a good antistatic effect is achieved.
Table 3 results of conductivity tests of examples 1 to 5 and comparative examples 1 to 3
| Sample(s) | Conductivity (s/cm) |
| Example 1 | 1.52E-10 |
| Example 2 | 1.55E-10 |
| Example 3 | 1.12E-10 |
| Example 4 | 1.47E-10 |
| Example 5 | 1.33E-10 |
| Comparative example 1 | 1.71E-11 |
| Comparative example 2 | 5.23E-11 |
| Comparative example 3 | 2.54E-11 |
In conclusion, after the inorganic nano filler and the conductive filler are added, the mechanical property of the waterborne polyurethane is greatly improved, and the elongation at break is improved while the tensile strength is increased. Meanwhile, the graphene oxide and the PEDOT PSS are added to form a filler network structure, so that compared with the case that a certain filler is added alone, the elongation at break is higher, the mechanical property is improved, and in addition, the PEDOT PSS and the graphene oxide are added to improve the conductivity of the composite material and improve the antistatic property.
Claims (10)
1. An antistatic waterborne polyurethane coating material is characterized in that:
the antistatic aqueous polyurethane coating material is prepared from raw materials including an aqueous polyurethane solution, a water-dispersible inorganic nano filler and a water-dispersible conductive organic filler;
the mass ratio of the water-based polyurethane to the water-dispersible inorganic nano filler to the water-dispersible conductive organic filler is 100:0.1 to 5:0.1 to 5.
2. The antistatic aqueous polyurethane coating material as claimed in claim 1, wherein:
the mass ratio of the water-based polyurethane to the water-dispersible inorganic nano filler to the water-dispersible conductive organic filler is 100:0.1 to 0.5:0.1 to 0.5.
3. The antistatic aqueous polyurethane coating material as claimed in claim 1, wherein:
the aqueous polyurethane solution is a cationic aqueous polyurethane solution or an anionic aqueous polyurethane solution.
4. The antistatic aqueous polyurethane coating material as claimed in claim 1, wherein:
the solid content of the aqueous polyurethane solution is 10-25%.
5. The antistatic aqueous polyurethane coating material as claimed in claim 1, wherein:
the total water content of the mixed solution of the aqueous polyurethane solution, the water dispersible inorganic nano filler and the water dispersible conductive organic filler is 70-90%, and preferably 80-85%.
6. The antistatic aqueous polyurethane coating material as claimed in claim 1, wherein:
the water-dispersible inorganic nano filler is at least one of graphene oxide, hydroxyl modified two-dimensional inorganic nano filler and carboxyl modified two-dimensional inorganic nano filler.
7. The antistatic aqueous polyurethane coating material as claimed in claim 1, wherein:
the hydroxyl modified two-dimensional inorganic nano filler is boron nitride; and/or the presence of a gas in the gas,
the carboxyl modified two-dimensional inorganic nano filler is a silicon dioxide nanosphere.
8. The antistatic aqueous polyurethane coating material as claimed in claim 1, wherein:
the water-dispersible conductive filler is poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid.
9. A method for preparing the antistatic aqueous polyurethane coating material as claimed in one of claims 1 to 8, characterized in that the method comprises:
and uniformly mixing the raw materials according to the proportion, defoaming and drying to obtain the antistatic waterborne polyurethane coating material.
10. The method for preparing the antistatic aqueous polyurethane coating material as claimed in claim 9, wherein:
the mixing temperature is 20-60 ℃;
the drying temperature is 45-100 ℃.
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