CN115746679B - Heat-conducting water vapor barrier coating, coating stock solution and preparation method and application thereof - Google Patents
Heat-conducting water vapor barrier coating, coating stock solution and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to the technical field of high polymer materials, in particular to a heat-conducting water vapor barrier coating, a coating stock solution and a preparation method and application thereof, wherein the coating stock solution comprises the following raw materials in percentage by mass: 15% -40% of base material resin; 5% -15% of flaky filler; 2% -5% of spherical filler; 50% -75% of solvent; 0.1 to 0.5 percent of silane coupling agent; 0.1 to 0.5 percent of curing agent. The coating provided by the invention has high heat conduction performance, excellent water vapor barrier performance, excellent ageing resistance, environmental stability and temperature resistance.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a heat-conducting water vapor barrier coating, a coating stock solution, a preparation method and application thereof.
Background
The polymer material has the characteristics of light weight, good toughness, easy processing and the like, so that the application range and the field of the polymer material are continuously expanded, wherein the polymer material is used for the packaging, encapsulation and protection industries, such as the packaging of foods, medicines and beverages, the encapsulation of electronic chips and other electronic materials, the protection of OLED and solar cells and the like. The pure polymer material is composed of polymerized units and is permeable in nature. The process of permeation of small molecular substances into polymeric materials can generally be divided into four stages: four processes, 1) adsorption, 2) dissolution, 3) diffusion and 4) desorption. Wherein, the permeation of water vapor molecules can cause the oxidation corrosion of the base material and the reduction of the working efficiency of the device, and the performance of the pure polymer protective material cannot meet the requirements.
In addition, the high polymer material in the electronic material has poor heat conducting performance, so that the temperature rise is often generated in use, and the performance of the high polymer material is influenced. As the heat carrier inside the substance mainly comprises molecules, electrons, phonons, photons, etc. Phonons are energy quanta of simple harmonic vibration in lattice vibration, and are main carriers for heat transfer of high polymer materials. However, the irregular entanglement of the molecular chains of the polymer material, high relative molecular mass, non-uniformity, molecular vibration and incompatibility of lattice vibration make it impossible to well utilize phonon seat carriers to achieve the effect of high heat transfer. The heat conductivity coefficient of the high polymer material is generally about 0.2W/m.K, and the heat dissipation requirement of industrial application can not be met.
In the prior art, the application number is 201711002438.3, and the invention is a solvent type water vapor barrier coating, a coating stock solution, a preparation method and an application thereof. The requirements of improving the water vapor barrier property and the heat conductivity of the polymer material at present cannot be met at the same time.
Disclosure of Invention
Therefore, the invention aims to provide a heat-conducting water vapor barrier coating, a coating stock solution, a preparation method and application thereof, which are used for improving the water vapor barrier property and the heat conductivity of a high polymer material, and have excellent ageing resistance, environmental stability and temperature resistance.
Based on the purposes, the invention provides a heat-conducting water vapor barrier coating stock solution, which comprises the following raw materials in percentage by mass:
the mass percentage of the base resin may be 15%,16%,17%,18%,19%, 20%,21%,22%,23%,24%,25%,26%,27%,28%,29%,30%,31%, 32%,33%,34%,35%,36%,37%,38%,39% or 40%, etc., the mass percentage of the plate-like filler may be 5%,6%,7%,8%,9%,10%,11%,12%,13%,14%,15%, etc., the mass percentage of the spherical filler may be 2%,3%,4%,5%, etc., the mass percentage of the solvent may be 50%,55%,60%,65%,70%,75%, etc., the mass percentage of the silane coupling agent and the curing agent may be 0.1%,0.2%,0.3%,0.4%,0.5%, etc., but the present invention is not limited to the above-listed values, and other values not listed in the above numerical ranges may be equally applicable.
Optionally, the substrate resin is any one or a combination of at least two of polyester resin, unsaturated resin, alkyd resin or polyurethane; classical but non-limiting examples of such combinations are: a combination of polyester resin and polyurethane, a combination of unsaturated resin and alkyd resin, a combination of polyester resin, unsaturated resin and alkyd resin.
The number average molecular weight of the base resin is preferably 3000 to 35000, such as 3000, 5000, 7000, 10000, 15000, 20000, 25000, 30000 or 35000, etc., but is not limited to the recited values, and other non-recited values within the range of the recited values are used as well.
The solvent is any one or the combination of at least two of ethyl acetate, butyl acetate, tetrahydrofuran or butanone. Typical but non-limiting examples of such combinations are: ethyl acetate and butyl acetate, ethyl acetate and butanone, butanone and tetrahydrofuran, ethyl acetate, butyl acetate and butanone, and the like.
Preferably, the mass ratio of the two solvent combinations is 1:2,1:3,1:4, and the mass ratio of the three solvent combinations is 1:1:3.
Optionally, the platy filler is any one or a combination of at least two of boron nitride, graphene, mxene or graphite. Classical but non-limiting examples of such combinations are: a combination of boron nitride and graphene, a combination of boron nitride and graphite, a combination of Mxene and graphene, or a combination of boron nitride, graphene, and Mxene.
Optionally, the spherical filler is any one or a combination of at least two of aluminum oxide, aluminum nitride and silicon carbide.
Preferably, the mass ratio of the platy filler to the spherical filler is one of 1:1,2:1, 3:1.
The curing agent is isocyanate curing agent, and the isocyanate curing agent comprises any one or a combination of at least two of TDI, MDI, HDI, XDI and IPDI. Typical but non-limiting examples of such combinations are: a combination of TDI and MDI, a combination of TDI and HDI, a combination of MDI and XDI, a combination of MDI and IPDI, or a combination of TDI, MDI and IPDI, etc.
The silane coupling agent is any one or the combination of at least two of KH550, KH560, KH570, OFS-6341, KBM403, KBM4803 or KBM 5803. Typical but non-limiting examples of such combinations are: a combination of KH550 and KH560, a combination of KH560 and KH570, a combination of OFS-6341 and KH570, a combination of KBM403 and KM4803, a combination of KH570 and KBM5803, and the like.
The invention also provides a preparation method of the heat-conducting water vapor barrier coating stock solution, which comprises the following steps:
(1) Placing the flaky filler, the spherical filler and the silane coupling agent with the formula amount into a ball mill for ball milling to obtain mixed powder;
(2) And (3) uniformly mixing the mixed powder obtained in the step (1) with the base material resin, the solvent and the curing agent to obtain the heat-conducting water vapor barrier coating stock solution.
According to the invention, the flaky filler, the spherical filler and the silane coupling agent are added into the ball mill at the same time, the spherical filler is used as a substitute of zirconium beads in the traditional ball mill, the flaky filler is directly subjected to ball milling, so that the flaky filler is peeled off, and the added silane coupling agent can modify the surface of the filler, so that the filler can be better combined with resin, the interface thermal resistance can be reduced, the water vapor barrier capability can be improved, more heat conduction micro points can be provided by the spherical filler, and the heat conduction capability of the prepared coating can be further improved.
Preferably, the ball milling speed in the step (1) is 500-100rpm, such as 500rpm,600rpm, 700rpm,800rpm,900rpm or 1000rpm, etc., but not limited to the recited values, and other non-recited values within the range are equally applicable.
Preferably, the reaction time in the step (1) is 12-48h, such as 12h,18h,24h,30h,36h, 42h or 48h, etc., but is not limited to the recited values, and other non-recited values within the range are equally applicable.
Preferably, the stirring speed in the step (2) is 200-500rpm, such as 200rpm,300rpm, 400rpm or 500rpm, etc., but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the reaction time in the step (2) is 2-8h, such as 2h,3h,4h,6h, 7h or 8h, etc., but is not limited to the recited values, and other non-recited values within the range are equally applicable.
The invention also provides a heat-conducting water vapor barrier coating, which is obtained by coating the coating stock solution according to any one of claims 1-6 on a substrate and volatilizing a solvent.
Optionally, the substrate is any one of PET, PBT, PP or PE.
Optionally, the method for coating the coating stock solution on the surface of the substrate comprises any one of dip coating, spin coating, knife coating and spray coating.
The solvent volatilizing method may be that the solvent volatilizes naturally at normal temperature or that the base material coated with the stock solution is dried in an oven at 80 deg.c for 10-30 min.
The invention also provides application of the heat-conducting water vapor barrier coating in the fields of solar cells, OLED protection, electronic material encapsulation and packaging.
The invention has the beneficial effects that:
(1) The heat-conducting water vapor barrier coating is prepared by adding the filler in a blending way and combining other raw materials, so that the coating has good heat conduction performance and excellent water vapor barrier performance, and also has excellent ageing resistance, environmental stability, boiling resistance and temperature resistance, the water vapor transmission amount is reduced by 0-20% and the heat conduction performance is reduced by 0-10% after PCT high-pressure accelerated ageing, high-temperature high-humidity and temperature change experiments.
(2) The heat-conducting water vapor barrier coating has good heat-conducting property, and the heat-conducting coefficient is more than 0.8W/m.K.
(3) The heat-conducting water vapor barrier coating has excellent water vapor barrier performance, and the water vapor transmission rate is 0.5-2g/m 2 ·day。
(4) The heat-conducting water vapor barrier coating disclosed by the invention is environment-friendly in raw materials, green and environment-friendly, and has a good industrial application prospect.
Drawings
In order to more clearly illustrate the invention or the technical solutions of the prior art, the drawings which are used in the description of the embodiments or the prior art will be briefly described, it being obvious that the drawings in the description below are only of the invention and that other drawings can be obtained from them without inventive effort for a person skilled in the art.
FIG. 1 is a TEM image of boron nitride after ball milling according to the present invention;
FIG. 2 is a surface optical microscope image of a pure substrate resin coating, a boron nitride single filler/resin coating, a boron nitride, aluminum oxide composite filler/resin coating of the present invention;
FIG. 3 is a cross-sectional scanning electron microscope image of a boron nitride, aluminum oxide composite filler/resin coating, aluminum oxide single filler/resin coating, boron nitride single filler/resin coating of the present invention.
Detailed Description
The present invention will be further described in detail with reference to specific embodiments in order to make the objects, technical solutions and advantages of the present invention more apparent.
It is to be noted that unless otherwise defined, technical or scientific terms used herein should be taken in a general sense as understood by one of ordinary skill in the art to which the present invention belongs. The word "comprising" or "comprises", and the like, means that elements or items preceding the word are included in the element or item listed after the word and equivalents thereof, but does not exclude other elements or items.
Example 1
The preparation method of the heat-conducting water vapor barrier coating stock solution comprises the following steps:
(1) 6g of flaky boron nitride, 2g of spherical alumina and 570.1 g of KH are put into a ball mill for ball milling, and the mixed powder is obtained after ball milling for 12 hours at 1000 rpm.
(2) And (3) stirring 16.4g of the mixed powder obtained in the step (1), 75g of ethyl acetate and 0.5g of TDI at 200rpm for 8 hours to obtain the heat-conducting water vapor barrier coating stock solution.
And (3) spreading the prepared heat-conducting water vapor barrier water vapor coating stock solution on a PET film with the thickness of 125 mu m, and volatilizing the solvent to obtain the heat-conducting water vapor barrier coating.
Example 2
The preparation method of the heat-conducting water vapor barrier coating stock solution comprises the following steps:
(1) 5g of flaky graphene, 5g of spherical silicon carbide and 0.5g of KH560 are put into a ball mill for ball milling, and ball milling is carried out for 48 hours at 500rpm, so as to obtain mixed powder.
(2) And (3) stirring 39.4g of the mixed powder obtained in the step (1), 50g of butyl acetate and 0.1g of MDI at 500rpm for 2 hours to obtain the heat-conducting water vapor barrier coating stock solution.
And (3) spreading the prepared heat-conducting water vapor barrier coating stock solution on a 125 mu m PBT film, and drying at 80 ℃ for 10min to obtain the heat-conducting water vapor barrier coating.
Example 3
The preparation method of the heat-conducting water vapor barrier coating stock solution comprises the following steps:
(1) 15g of flake graphite, 5g of spherical silicon carbide and 0.2g of OFS-6341 are put into a ball mill for ball milling, and ball milling is carried out for 24 hours at 700rpm, so as to obtain mixed powder.
(2) And (3) stirring 15g of the mixed powder obtained in the step (1), 64.5g of butanone and 0.3g of MDI at 500rpm for 2 hours to obtain the heat-conducting water vapor barrier coating stock solution.
And (3) spreading the prepared heat-conducting water vapor barrier coating stock solution on a 125 mu m PP film, and drying at 80 ℃ for 30min to obtain the heat-conducting water vapor barrier coating.
Example 4
The preparation method of the heat-conducting water vapor barrier coating stock solution comprises the following steps:
(1) 10g of flaky boron nitride, 5g of spherical aluminum nitride and 0.4g of KH560 are put into a ball mill for ball milling, and ball milling is carried out for 24 hours at 700rpm, thus obtaining mixed powder.
(2) And (3) stirring 15g of the mixed powder obtained in the step (1), 69.2g of ethyl acetate and 0.4g of MDI at 300rpm for 6 hours to obtain the heat-conducting water vapor barrier coating stock solution.
And (3) spreading the prepared heat-conducting water vapor barrier water vapor coating stock solution on a 125 mu m PP film, and volatilizing the solvent to obtain the heat-conducting water vapor barrier coating.
Example 5
The preparation method of the heat-conducting water vapor barrier coating stock solution comprises the following steps:
(1) 6g of flaky boron nitride, 3g of spherical aluminum nitride and 403.5 g of KBM are put into a ball mill for ball milling, and ball milling is carried out for 24 hours at 700rpm, so as to obtain mixed powder.
(2) And (3) stirring 40g of the mixed powder obtained in the step (1), 40g of ethyl acetate, 10g of butyl acetate, 0.1g of XDI and 0.4g of IPDI for 4 hours at 400rpm to obtain the heat-conducting water vapor barrier coating stock solution.
And (3) spreading the prepared heat-conducting water vapor barrier coating stock solution on a 125 mu m PP film, and drying at 80 ℃ for 10min to obtain the heat-conducting water vapor barrier coating.
Example 6
The preparation method of the heat-conducting water vapor barrier coating stock solution comprises the following steps:
(1) 6g of flaky boron nitride, 3g of graphene, 2.5g of spherical aluminum nitride, 2.5g of spherical aluminum oxide, 560.3 g of KH and 0.1g of KH are put into a ball mill for ball milling, and ball milling is carried out for 24 hours at 700rpm, so as to obtain mixed powder.
(2) And (3) stirring 20g of the mixed powder obtained in the step (1), 15g of polyurethane, 50.2g of ethyl acetate and 0.4g of MDI at 300rpm for 6 hours to obtain the heat-conducting water vapor barrier coating stock solution.
And (3) spreading the prepared heat-conducting water vapor barrier water vapor coating stock solution on a PET film with the thickness of 125 mu m, and volatilizing the solvent to obtain the heat-conducting water vapor barrier coating.
Example 7
The preparation method of the heat-conducting water vapor barrier coating stock solution comprises the following steps:
(1) 6g of flaky boron nitride, 3g of graphite, 2.5g of spherical silicon carbide, 2.5g of spherical alumina and OFS-6341 0.3g,KH570 0.1g are put into a ball mill for ball milling, and ball milling is carried out for 36 hours at 600rpm, so as to obtain mixed powder.
(2) And (3) stirring 20g of the mixed powder obtained in the step (1), 15g of polyurethane, 50.2g of ethyl acetate, 0.2g of MDI and 0.2g of TDI for 55h at 400rpm to obtain the heat-conducting water vapor barrier coating stock solution.
And (3) spreading the prepared heat-conducting water vapor barrier coating stock solution on a 125 mu m PP film, and drying at 80 ℃ for 30min to obtain the heat-conducting water vapor barrier coating.
Comparative example 1
The preparation method comprises the steps of stirring 16.4g of polyester resin, 75g of ethyl acetate and 0.5g of TDI at 200rpm for 8 hours to obtain the heat-conducting water vapor barrier coating stock solution.
And (3) spreading the prepared heat-conducting water vapor barrier water vapor coating stock solution on a PET film with the thickness of 125 mu m, and volatilizing the solvent to obtain the heat-conducting water vapor barrier coating.
Comparative example 2
(1) 8g of flaky boron nitride and 570.1 g of KH are put into a ball mill for ball milling, and the mixed powder is obtained after ball milling for 12 hours at 1000 rpm.
(2) And (3) stirring 16.4g of the mixed powder obtained in the step (1), 75g of ethyl acetate and 0.5g of TDI at 200rpm for 8 hours to obtain the heat-conducting water vapor barrier coating stock solution.
And (3) spreading the prepared heat-conducting water vapor barrier water vapor coating stock solution on a PET film with the thickness of 125 mu m, and volatilizing the solvent to obtain the heat-conducting water vapor barrier coating.
Comparative example 3
(1) Spherical alumina 8g and KH 570.1 g were put into a ball mill for ball milling at 1000rpm for 12 hours to obtain mixed powder.
(2) And (3) stirring 16.4g of the mixed powder obtained in the step (1), 75g of ethyl acetate and 0.5g of TDI at 200rpm for 8 hours to obtain the heat-conducting water vapor barrier coating stock solution.
And (3) spreading the prepared heat-conducting water vapor barrier water vapor coating stock solution on a PET film with the thickness of 125 mu m, and volatilizing the solvent to obtain the heat-conducting water vapor barrier coating.
The properties of the coatings obtained in examples 1 to 7 and comparative examples 1 to 3 were examined by an accelerated aging test, a constant temperature and humidity test and a high and low temperature test. The accelerated aging test is carried out by using a PCT high-pressure accelerated aging tester of Hongyuan in Taiwan, and then carried out for 48 hours at the temperature of 121 ℃ and the pressure of 0.2 MPa. The constant temperature and humidity experiment was carried out using a constant temperature and humidity oven of sepec, and then placed at 85℃and 85% RH for 2000 hours. The high and low temperature experiment was performed using a high and low temperature alternating damp heat test chamber of espec at-40 ℃ to 80 ℃ with 3 hours as one cycle for a total of 200 cycles. The Water Vapor Transmission Rate (WVTR) is measured using Mocon water vapor transmission rate tester PERMATRAN-W1/50, U.S.A. The thermal conductivity was measured using a Siam Xiaxi electronic TC3000E thermal conductivity tester. The hydrolysis resistance test was 95℃water boiling for 24 hours. The test results are shown in tables 1 and 2.
TABLE 1
TABLE 2
TABLE 3 Table 3
According to Table 1As can be seen from the results, the heat conductive water vapor barrier coatings obtained in examples 1 to 7 have excellent vapor barrier properties and good heat conductive properties, and a WVTR of 0.5 to 2g/m 2 Day, after various aging tests, WVTR is reduced to 0-20%, the heat conductivity coefficient is 0.8-1.55W/m.K, after various aging tests, the heat conductivity coefficient is reduced to 0-10%, and the coating has excellent heat resistance and aging resistance.
From the results of Table 2, it can be seen that comparative example 1 uses only pure base resin, WVTR is greatly reduced after aging test, heat conduction property is slightly reduced, comparative example 2 uses only flake boron nitride as filler to prepare coating, water vapor barrier property and heat conduction property are lower than those of example, comparative example 3 uses only spherical alumina as filler to prepare coating, water vapor barrier property of coating is improved only a little, and heat conduction property is improved a little.
Those of ordinary skill in the art will appreciate that: the discussion of any of the embodiments above is merely exemplary and is not intended to suggest that the scope of the invention (including the claims) is limited to these examples; the technical features of the above embodiments or in the different embodiments may also be combined within the idea of the invention, the steps may be implemented in any order and there are many other variations of the different aspects of the invention as described above, which are not provided in detail for the sake of brevity.
The present invention is intended to embrace all such alternatives, modifications and variances which fall within the broad scope of the appended claims. Therefore, any omission, modification, equivalent replacement, improvement, etc. of the present invention should be included in the scope of the present invention.
Claims (8)
1. The heat-conducting water vapor barrier coating stock solution is characterized by comprising the following raw materials in percentage by mass:
15% -40% of base material resin;
5% -15% of flaky filler;
2% -5% of spherical filler;
50% -75% of a solvent;
0.1% -0.5% of silane coupling agent;
0.1% -0.5% of curing agent;
the coating stock solution is formed by uniformly mixing mixed powder with base material resin, a solvent and a curing agent, wherein the mixed powder is obtained by ball milling a flaky filler, a spherical filler and a silane coupling agent in a ball mill, the spherical filler is used as a substitute of zirconium beads in the traditional ball mill, the flaky filler is directly ball milled to strip the flaky filler, the flaky filler is any one or a combination of at least two of boron nitride, graphene, mxene and graphite, and the spherical filler is any one or a combination of at least two of aluminum oxide, aluminum nitride and silicon carbide.
2. The thermally conductive water vapor barrier coating stock solution of claim 1, wherein the substrate resin is any one or a combination of at least two of a polyester resin, an unsaturated resin, an alkyd resin, or polyurethane; the solvent is any one or the combination of at least two of ethyl acetate, butyl acetate, tetrahydrofuran or butanone.
3. The thermally conductive water vapor barrier coating stock solution of claim 1, wherein the curing agent is an isocyanate-type curing agent comprising any one or a combination of at least two of TDI, MDI, HDI, XDI or IPDI.
4. The thermally conductive water vapor barrier coating stock solution of claim 1, wherein the silane coupling agent is any one or a combination of at least two of KH550, KH560, KH570, OFS-6341, KBM403, KBM4803, or KBM 5803.
5. The method for preparing a heat conductive water vapor barrier coating stock solution according to any one of claims 1 to 4, comprising the steps of:
(1) Placing the flaky filler, the spherical filler and the silane coupling agent with the formula amount into a ball mill for ball milling to obtain mixed powder;
(2) And (3) uniformly mixing the mixed powder obtained in the step (1) with the base material resin, the solvent and the curing agent to obtain the heat-conducting water vapor barrier coating stock solution.
6. A thermally conductive water vapor barrier coating, characterized in that said coating is obtained by applying the coating stock solution according to any one of claims 1-4 to a substrate, after which the solvent is evaporated.
7. The thermally conductive water vapor barrier coating of claim 6, wherein the substrate is either PET, PBT, PP or PE.
8. Use of the thermally conductive moisture barrier coating of claim 6 or 7 in the fields of solar cells, OLED protection, electronics packaging and packaging.
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