CN117210084A - Low-silicon release agent for MLCC, preparation method thereof and release film - Google Patents
Low-silicon release agent for MLCC, preparation method thereof and release film Download PDFInfo
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- CN117210084A CN117210084A CN202311210129.0A CN202311210129A CN117210084A CN 117210084 A CN117210084 A CN 117210084A CN 202311210129 A CN202311210129 A CN 202311210129A CN 117210084 A CN117210084 A CN 117210084A
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- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 74
- 239000010703 silicon Substances 0.000 title claims abstract description 74
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title abstract description 17
- 229920002545 silicone oil Polymers 0.000 claims abstract description 59
- QWDQYHPOSSHSAW-UHFFFAOYSA-N 1-isocyanatooctadecane Chemical compound CCCCCCCCCCCCCCCCCCN=C=O QWDQYHPOSSHSAW-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000003054 catalyst Substances 0.000 claims abstract description 23
- 239000004640 Melamine resin Substances 0.000 claims abstract description 20
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 20
- 239000002904 solvent Substances 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 51
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 48
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 46
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 29
- JOXIMZWYDAKGHI-UHFFFAOYSA-N p-toluenesulfonic acid Substances CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 23
- 239000004925 Acrylic resin Substances 0.000 claims description 16
- 229920000178 Acrylic resin Polymers 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 16
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 14
- 239000011248 coating agent Substances 0.000 claims description 14
- 238000000576 coating method Methods 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 12
- 229920002799 BoPET Polymers 0.000 claims description 10
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical group CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 10
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 10
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 8
- 230000002378 acidificating effect Effects 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 229920000570 polyether Polymers 0.000 claims description 8
- 229920000728 polyester Polymers 0.000 claims description 7
- 239000003377 acid catalyst Substances 0.000 claims description 3
- 125000005489 p-toluenesulfonic acid group Chemical group 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 5
- 229920005989 resin Polymers 0.000 abstract description 5
- 239000011347 resin Substances 0.000 abstract description 5
- 150000001335 aliphatic alkanes Chemical class 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract description 3
- 230000003746 surface roughness Effects 0.000 abstract description 3
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- 230000002776 aggregation Effects 0.000 abstract description 2
- 239000000919 ceramic Substances 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 11
- 239000012046 mixed solvent Substances 0.000 description 7
- 229920000139 polyethylene terephthalate Polymers 0.000 description 7
- -1 polyethylene terephthalate Polymers 0.000 description 7
- 239000005020 polyethylene terephthalate Substances 0.000 description 7
- 239000002002 slurry Substances 0.000 description 4
- 238000005303 weighing Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 239000003985 ceramic capacitor Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229920003270 Cymel® Polymers 0.000 description 1
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 description 1
- JAUOIFJMECXRGI-UHFFFAOYSA-N Neoclaritin Chemical compound C=1C(Cl)=CC=C2C=1CCC1=CC=CN=C1C2=C1CCNCC1 JAUOIFJMECXRGI-UHFFFAOYSA-N 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 1
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- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical group NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 239000003960 organic solvent Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
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- 230000008023 solidification Effects 0.000 description 1
- 238000010345 tape casting Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
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- Laminated Bodies (AREA)
Abstract
The invention discloses a low-silicon release agent for MLCC, a preparation method thereof and a release film, which comprises the following raw material components in percentage by mass: 5-20% of modified silicone oil, 10-40% of melamine resin, 0.1-1% of catalyst, 0.2-2% of octadecyl isocyanate and the balance of solvent. According to the invention, octadecyl isocyanate is grafted through the reaction of-OH and-NCO groups on the long chain of modified silicone oil, and then the residual-OH and melamine resin on the long chain of silicone oil are cured to form a film; on the premise of ensuring lower stripping force, long-chain alkane improves the wettability of the release agent to the base material, and avoids the problem that the surface roughness of the release layer is increased due to protrusion caused by aggregation of various resins during drying. The release film disclosed by the invention has the smoothness and the peelability of the MLCC release film, is excellent in weather resistance and has a wide market application prospect.
Description
Technical Field
The invention relates to the field of MLCC release materials, in particular to a low-silicon release agent for an MLCC, a preparation method thereof and a release film.
Background
The MLCC is widely applied to circuits of automobile electronics, industrial automation, 5G communication due to the advantages of small volume, large capacitance, wide working voltage and working temperature range and the like, has functions of filtering, coupling, resonance, bypass and the like, brings considerable prospect for MLCC localization, and brings serious technical challenges. In the manufacturing process of the ceramic membrane, the MLCC release film directly contacts with ceramic slurry to play a role in bearing and stably stripping the ceramic plate, so that the suitability, roughness and cleanliness of the MLCC release film can directly influence the quality of an MLCC finished product. When the non-silicon release agent peels off the ceramic green sheet, the peeling force is larger, and the thin ceramic green sheet is damaged; the silicone release agent has a light release force but a relatively low residue, and poor wettability to the substrate, resulting in an increased roughness of the MLCC release film. In the release layer containing the binder resin and the silicone resin, the solubility of the binder resin in an organic solvent and the surface tension of the solution are greatly different, so that the phase becomes poor when dried, and the resins aggregate to form protrusions, and the roughness of the surface of the release layer is increased. When ceramic green sheets having a thickness of 1.0 μm or less, or even 0.6 μm or less are molded, even if these minute surface roughness increases, the failure rate of the laminated ceramic capacitor, which can cause pinholes or the like, is deteriorated, and therefore further smoothness and releasability are required.
Patent CN 112280085A discloses a low-roughness MLCC functional release film capable of being used in tape casting and a preparation method thereof, wherein a low-temperature cured silicone oil formula is adopted, so that a low-temperature cured release coating can be cured at a temperature below 110 ℃, and the heat shrinkage stability of the release film is ensured. However, the release layer has a low elastic modulus and is easily deformed during the peeling of the ceramic green sheet, and thus has problems of low release force and instability.
Patent CN 116063886a discloses a high temperature resistant non-silicon release material, a non-silicon release film and a preparation method thereof, wherein the non-silicon release film has the advantages of good high temperature resistance, small coating amount of release agent, low aging climbing rate of the release film, high aging residue rate and the like by regulating and controlling the proportion of high molecular weight acrylic resin and low molecular weight acrylic resin. However, the release force is large, the ceramic green sheet is difficult to peel from the release layer, and the requirement of the multilayer ceramic capacitor MLCC release film on low release force is difficult to be met.
Therefore, there is a need in the art for improvements that provide a more reliable solution.
Disclosure of Invention
The invention aims to solve the technical problem of providing a low-silicon release agent for MLCC, a preparation method thereof and a release film aiming at the defects in the prior art.
In order to solve the technical problems, the invention adopts the following technical scheme: the invention provides a low-silicon parting agent for MLCC, which comprises the following raw material components in percentage by mass: 5-20% of modified silicone oil, 10-40% of melamine resin, 0.1-1% of catalyst, 0.2-2% of octadecyl isocyanate and the balance of solvent.
Preferably, the modified silicone oil is one of polyether modified hydroxyl-containing silicone oil, polyester modified hydroxyl-containing silicone oil and acrylic resin modified hydroxyl-containing silicone oil.
Preferably, the molar ratio of-OH in the modified silicone oil to-NCO in the octadecyl isocyanate is 2:1 to 4:1.
preferably, the molar ratio of-OH in the modified silicone oil to-NCO in the octadecyl isocyanate is 2:1 or 3:1 or 4:1.
preferably, the catalyst comprises an organotin catalyst and an acidic catalyst.
Preferably, the organotin catalyst is dibutyl tin dilaurate, and the acidic catalyst is p-toluenesulfonic acid.
Preferably, the solvent is a mixture of butanone, isopropanol and toluene, and the butanone accounts for 10-40% of the total raw material, the isopropanol accounts for 5-10% of the total raw material, and the toluene accounts for 10-50% of the total raw material.
In a second aspect of the present invention, there is provided a method for preparing a low silicon release agent for an MLCC as described above, comprising the steps of:
mixing the modified silicone oil, the organotin catalyst, the octadecyl isocyanate and part of solvent, stirring for 15-60min, performing a prepolymerization reaction to ensure that-OH in the modified silicone oil and-NCO in the octadecyl isocyanate completely react, then adding melamine resin, an acidic catalyst and the rest of solvent, and stirring for 5-30min to obtain the low-silicon release agent for the MLCC.
Preferably, the preparation method of the low-silicon release agent for the MLCC comprises the following steps:
mixing the modified silicone oil, dibutyl tin dilaurate, octadecyl isocyanate and toluene, stirring for 15-60min, performing a prepolymerization reaction to enable-OH in the modified silicone oil and-NCO in the octadecyl isocyanate to completely react, then adding melamine resin, acid catalyst p-toluenesulfonic acid, butanone and isopropanol, and stirring for 5-30min to obtain the low-silicon release agent for MLCC.
In a third aspect of the present invention, there is provided a low silicon release film for an MLCC, which is prepared by: the low-silicon release agent for MLCC is uniformly coated on a PET film with the thickness of 25-100 mu m, the coating thickness is controlled to be 300-800nm, and the low-silicon release agent for MLCC is obtained by baking for 0.5-2min at the temperature of 110-130 ℃.
The beneficial effects of the invention are as follows:
the invention provides a low-silicon release agent for MLCC, a preparation method and a release film thereof, wherein the invention is characterized in that-OH on a long chain of modified silicone oil (polyether modified hydroxyl-containing silicone oil, polyester modified hydroxyl-containing silicone oil and acrylic resin modified hydroxyl-containing silicone oil) reacts with-NCO groups, octadecylisocyanate is grafted, and the residual-OH on the long chain of silicone oil and melamine resin are solidified to form a film; on the premise of ensuring lower stripping force, long-chain alkane improves the wettability of the release agent to the base material, and avoids the problem that the surface roughness of the release layer is increased due to protrusion caused by aggregation of various resins during drying;
the melamine resin in the release film structure can provide rigidity and solidification, the octadecyl isocyanate can provide flexibility and high wettability, and the modified silicone oil can provide flexibility and low stripping force, so that the release film disclosed by the invention has the smoothness and stripping property of the MLCC release film, is excellent in weather resistance and has a wide market application prospect.
Detailed Description
The present invention is described in further detail below with reference to examples to enable those skilled in the art to practice the same by referring to the description.
It will be understood that terms, such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
The test methods used in the following examples are conventional methods unless otherwise specified. The material reagents and the like used in the following examples are commercially available unless otherwise specified. The following examples were conducted under conventional conditions or conditions recommended by the manufacturer, without specifying the specific conditions. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The invention provides a low-silicon parting agent for MLCC, which comprises the following raw material components in percentage by mass: 5-20% of modified silicone oil, 10-40% of melamine resin, 0.1-1% of catalyst, 0.2-2% of octadecyl isocyanate and the balance of solvent.
In a preferred embodiment, the modified silicone oil is one of polyether modified hydroxyl-containing silicone oil, polyester modified hydroxyl-containing silicone oil, and acrylic resin modified hydroxyl-containing silicone oil.
In a preferred embodiment, the molar ratio of-OH in the modified silicone oil to-NCO in the octadecyl isocyanate is 2:1 to 4:1. further preferably, the molar ratio of-OH in the modified silicone oil to-NCO in the octadecyl isocyanate is 2:1 or 3:1 or 4:1.
in a preferred embodiment, the catalyst comprises an organotin catalyst and an acidic catalyst. Further preferably, the organotin catalyst is dibutyltin dilaurate and the acidic catalyst is p-toluenesulfonic acid.
In a preferred embodiment, the solvent is a mixture of butanone, isopropanol and toluene, and the butanone is 10% -40%, the isopropanol is 5% -10%, and the toluene is 10% -50% by mass of the total raw materials.
The invention also provides a preparation method of the low-silicon release agent for the MLCC, which comprises the following steps:
mixing the modified silicone oil, dibutyl tin dilaurate, octadecyl isocyanate and toluene, stirring for 15-60min, performing prepolymerization reaction to make-OH in the modified silicone oil and-NCO in the octadecyl isocyanate completely react, adding melamine resin, acid catalyst p-toluenesulfonic acid, butanone and isopropanol, and stirring for 5-30min to obtain the low-silicon release agent for MLCC.
The invention also provides a low-silicon release film for the MLCC, which is prepared by the following method: the low-silicon release agent for MLCC is uniformly coated on a PET film with the thickness of 25-100 mu m, the coating thickness is controlled to be 300-800nm, and the low-silicon release film for MLCC is obtained by baking for 0.5-2min at the temperature of 110-130 ℃.
The foregoing is a general inventive concept and the following detailed examples and comparative examples are provided on the basis thereof to further illustrate the invention.
In the following examples and comparative examples, the acrylic resin modified hydroxyl-containing silicone oil was BYK3700, pick chemistry; the polyether modified hydroxyl-containing silicone oil is BYK377 and is of Pick chemistry; the polyester modified hydroxyl-containing silicone oil is BYK370, pick chemistry; the melamine resin source is CYMEL XW 3106, allex.
Example 1
A preparation method of a low-silicon release agent for MLCC comprises the following steps:
40g of acrylic resin modified hydroxyl-containing silicone oil, 1.6g of octadecyl isocyanate (the molar ratio of-OH in the acrylic resin modified hydroxyl-containing silicone oil to-NCO in the octadecyl isocyanate is 4:1), 0.02g of dibutyltin dilaurate and 150g of toluene are accurately weighed and mixed, after being fully stirred for 30min, 158.4g of mixed solvent of butanone and isopropanol (the mass ratio of butanone to isopropanol is 2:1), 50g of melamine resin and 1g of p-toluenesulfonic acid are added, and the mixture is stirred and dispersed for 30min to obtain the low-silicon release agent for MLCC.
A low-silicon release film for MLCC, which is prepared by the following method: the prepared low-silicon release agent for MLCC is uniformly coated on a PET film (polyethylene terephthalate) with the thickness of 50 mu m, the coating thickness is controlled to be 500nm, and the mixture is placed in an oven and baked for 1min at 120 ℃ to obtain the low-silicon release film for MLCC.
Example 2
A preparation method of a low-silicon release agent for MLCC comprises the following steps:
40g of acrylic resin modified hydroxyl-containing silicone oil, 2.2g of octadecyl isocyanate (the molar ratio of-OH in the acrylic resin modified hydroxyl-containing silicone oil to-NCO in the octadecyl isocyanate is 3:1), 0.02g of dibutyltin dilaurate and 150g of toluene are accurately weighed and mixed, after the mixture is fully stirred for 30min, 157.8g of mixed solvent of butanone and isopropanol (the mass ratio of butanone to isopropanol is 2:1), 50g of melamine resin and 1g of p-toluenesulfonic acid are added, and the mixture is stirred and dispersed for 30min to obtain the low-silicon release agent for MLCC.
A low-silicon release film for MLCC, which is prepared by the following method: the prepared low-silicon release agent for MLCC is uniformly coated on a PET film (polyethylene terephthalate) with the thickness of 50 mu m, the coating thickness is controlled to be 500nm, and the mixture is placed in an oven and baked for 1min at 120 ℃ to obtain the low-silicon release film for MLCC.
Example 3
A preparation method of a low-silicon release agent for MLCC comprises the following steps:
40g of acrylic resin modified hydroxyl-containing silicone oil, 3.2g of octadecyl isocyanate (the molar ratio of-OH in the acrylic resin modified hydroxyl-containing silicone oil to-NCO in the octadecyl isocyanate is 2:1), 0.02g of dibutyltin dilaurate and 150g of toluene are accurately weighed and mixed, after the mixture is fully stirred for 30min, 160g of mixed solvent of butanone and isopropanol (the mass ratio of butanone to isopropanol is 2:1), 50g of melamine resin and 1g of p-toluenesulfonic acid are added, and the mixture is stirred and dispersed for 30min to obtain the low-silicon release agent for MLCC.
A low-silicon release film for MLCC, which is prepared by the following method: the prepared low-silicon release agent for MLCC is uniformly coated on a PET film (polyethylene terephthalate) with the thickness of 50 mu m, the coating thickness is controlled to be 500nm, and the mixture is placed in an oven and baked for 1min at 120 ℃ to obtain the low-silicon release film for MLCC.
Example 4
A preparation method of a low-silicon release agent for MLCC comprises the following steps:
40g of polyether modified hydroxyl-containing silicone oil, 2.4g of octadecyl isocyanate (the molar ratio of-OH in the acrylic resin modified hydroxyl-containing silicone oil to-NCO in the octadecyl isocyanate is 4:1), 0.02g of dibutyltin dilaurate and 150g of toluene are accurately weighed and mixed, after being fully stirred for 30min, 157.6g of mixed solvent of butanone and isopropanol (the mass ratio of butanone to isopropanol is 2:1), 50g of melamine resin and 1g of p-toluenesulfonic acid are added, and the mixture is stirred and dispersed for 30min to obtain the low-silicon release agent for MLCC.
A low-silicon release film for MLCC, which is prepared by the following method: the prepared low-silicon release agent for MLCC is uniformly coated on a PET film (polyethylene terephthalate) with the thickness of 50 mu m, the coating thickness is controlled to be 500nm, and the mixture is placed in an oven and baked for 1min at 120 ℃ to obtain the low-silicon release film for MLCC.
Comparative example 1
A preparation method of a low-silicon release agent for MLCC comprises the following steps:
accurately weighing 40g of acrylic resin modified hydroxyl silicone oil and 150g of toluene, mixing, fully stirring for 30min, adding 160g of mixed solvent of butanone and isopropanol (the mass ratio of butanone to isopropanol is 2:1), 50g of melamine resin and 1g of p-toluenesulfonic acid, and stirring and dispersing for 30min to obtain the low-silicon release agent for MLCC.
A low-silicon release film for MLCC, which is prepared by the following method: the prepared low-silicon release agent for MLCC is uniformly coated on a PET film (polyethylene terephthalate) with the thickness of 50 mu m, the coating thickness is controlled to be 500nm, and the mixture is placed in an oven and baked for 1min at 120 ℃ to obtain the low-silicon release film for MLCC.
Comparative example 2
A preparation method of a low-silicon release agent for MLCC comprises the following steps:
accurately weighing 40g of polyether modified hydroxyl-containing silicone oil and 150g of toluene, mixing, fully stirring for 30min, adding 160g of mixed solvent of butanone and isopropanol (the mass ratio of butanone to isopropanol is 2:1), 50g of melamine resin and 1g of p-toluenesulfonic acid, and stirring and dispersing for 30min to obtain the low-silicon release agent for MLCC.
A low-silicon release film for MLCC, which is prepared by the following method: the prepared low-silicon release agent for MLCC is uniformly coated on a PET film (polyethylene terephthalate) with the thickness of 50 mu m, the coating thickness is controlled to be 500nm, and the mixture is placed in an oven and baked for 1min at 120 ℃ to obtain the low-silicon release film for MLCC.
Comparative example 3
A preparation method of a low-silicon release agent for MLCC comprises the following steps:
accurately weighing 40g of polyester modified hydroxyl-containing silicone oil and 150g of toluene, mixing, fully stirring for 30min, adding 160g of mixed solvent of butanone and isopropanol (the mass ratio of butanone to isopropanol is 2:1), 50g of melamine resin and 1g of p-toluenesulfonic acid, and stirring and dispersing for 30min to obtain the low-silicon release agent for MLCC.
A low-silicon release film for MLCC, which is prepared by the following method: the prepared low-silicon release agent for MLCC is uniformly coated on a PET film (polyethylene terephthalate) with the thickness of 50 mu m, the coating thickness is controlled to be 500nm, and the mixture is placed in an oven and baked for 1min at 120 ℃ to obtain the low-silicon release film for MLCC.
The MLCCs prepared in examples 1-4 and comparative examples 1-3 were tested with low silicon release films for the following performance tests:
(1) And (3) measuring the roughness of the release film: the roughness of the release film was measured by a white light interferometer, the area surface average roughness (Sa) was measured 5 times as an average value, and the maximum protrusion height (Rp) was measured 7 times as a maximum value of 5 times other than the maximum value and the minimum value.
(2) Peel force measurement:
preparing a ceramic green sheet: 38.3g of toluene, 38.3g of ethanol, 64.8g of barium titanate, 6.5g of polyvinyl butyral and 3.3g of dioctyl phthalate are weighed, stirred, mixed and dispersed for 60 minutes by using a ball mill with 0.5 mm-diameter glass beads as a dispersion medium, so as to obtain ceramic slurry.
Coating ceramic slurry on a release surface of the obtained release film sample by using a coater, enabling the thickness of the slurry to be 10 micrometers, and drying for 1min at 90 ℃ to form a ceramic green sheet; after charge was removed from the obtained release film with a ceramic green sheet, the release film was cut into strips 30mm wide, and the strips were peeled at a peeling angle of 90 degrees and a peeling speed of 10m/min, and the peeling force was measured.
The test results are shown in table 1 below:
TABLE 1
| Peel force (mN/mm 2) | Sa(nm) | Rp(nm) | |
| Example 1 | 1.5 | 0.9 | 39 |
| Example two | 1.6 | 0.9 | 36 |
| Example III | 1.6 | 0.8 | 37 |
| Example IV | 1.5 | 0.9 | 36 |
| Example five | 1.5 | 0.9 | 36 |
| Comparative example one | 1.5 | 1.8 | 64 |
| Comparative example two | 1.6 | 2.0 | 59 |
| Comparative example three | 1.5 | 2.3 | 46 |
As can be seen from the test data of examples 1 to 4 and comparative examples 1 to 3, in comparison with comparative examples 1 to 4, by grafting octadecylisocyanate onto the long chain-OH of the modified silicone oil (polyether modified hydroxyl-containing silicone oil, polyester modified hydroxyl-containing silicone oil, acrylic resin modified hydroxyl-containing silicone oil), the roughness can be greatly reduced while maintaining the lower peeling force of the ceramic film, and the wettability of the release agent to the substrate is improved mainly thanks to the long chain alkane.
Although embodiments of the present invention have been disclosed above, it is not limited to the use of the description and embodiments, it is well suited to various fields of use for the invention, and further modifications may be readily apparent to those skilled in the art, and accordingly, the invention is not limited to the particular details without departing from the general concepts defined in the claims and the equivalents thereof.
Claims (10)
1. The low-silicon parting agent for the MLCC is characterized by comprising the following raw material components in percentage by mass: 5-20% of modified silicone oil, 10-40% of melamine resin, 0.1-1% of catalyst, 0.2-2% of octadecyl isocyanate and the balance of solvent.
2. The low-silicon release agent for MLCCs of claim 1, wherein said modified silicone oil is one of polyether modified hydroxyl-containing silicone oil, polyester modified hydroxyl-containing silicone oil, and acrylic resin modified hydroxyl-containing silicone oil.
3. The low silicon release agent for MLCCs as claimed in claim 2, wherein a molar ratio of-OH in said modified silicone oil to-NCO in octadecyl isocyanate is 2:1 to 4:1.
4. the low silicon release agent for MLCCs as claimed in claim 3, wherein a molar ratio of-OH in said modified silicone oil to-NCO in octadecyl isocyanate is 2:1 or 3:1 or 4:1.
5. the low silicon release agent for MLCCs of claim 1, wherein said catalyst comprises an organotin catalyst and an acidic catalyst.
6. The low silicon release agent for MLCC according to claim 5, wherein the organotin catalyst is dibutyltin dilaurate and the acidic catalyst is p-toluenesulfonic acid.
7. The low silicon release agent for MLCCs as claimed in claim 1, wherein said solvent is a mixture of butanone, isopropyl alcohol and toluene, and the butanone is 10% -40%, isopropyl alcohol is 5% -10%, toluene is 10% -50% by mass of the total raw material.
8. A method for preparing the low silicon release agent for MLCCs as described in any one of claims 5 to 7, comprising the steps of:
mixing the modified silicone oil, the organotin catalyst, the octadecyl isocyanate and part of solvent, stirring for 15-60min, performing a prepolymerization reaction to ensure that-OH in the modified silicone oil and-NCO in the octadecyl isocyanate completely react, then adding melamine resin, an acidic catalyst and the rest of solvent, and stirring for 5-30min to obtain the low-silicon release agent for the MLCC.
9. The method for preparing a low silicon release agent for an MLCC according to claim 8, comprising the steps of:
mixing the modified silicone oil, dibutyl tin dilaurate, octadecyl isocyanate and toluene, stirring for 15-60min, performing a prepolymerization reaction to enable-OH in the modified silicone oil and-NCO in the octadecyl isocyanate to completely react, then adding melamine resin, acid catalyst p-toluenesulfonic acid, butanone and isopropanol, and stirring for 5-30min to obtain the low-silicon release agent for MLCC.
10. The low-silicon release film for the MLCC is characterized by being prepared by the following method: uniformly coating the low-silicon release agent for MLCC according to any one of claims 1-7 on a PET film with the thickness of 25-100 μm, controlling the coating thickness to 300-800nm, and baking at 110-130 ℃ for 0.5-2min to obtain the low-silicon release film for MLCC.
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| CN116535913A (en) * | 2023-03-22 | 2023-08-04 | 香洋新材料（江苏）有限公司 | Thermal transfer release for digital printing and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116535913A (en) * | 2023-03-22 | 2023-08-04 | 香洋新材料（江苏）有限公司 | Thermal transfer release for digital printing and preparation method thereof |
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