CN115322612A - 无机填料分散液、超疏水绝缘耐磨涂料及制备方法 - Google Patents
无机填料分散液、超疏水绝缘耐磨涂料及制备方法 Download PDFInfo
- Publication number
- CN115322612A CN115322612A CN202211269719.6A CN202211269719A CN115322612A CN 115322612 A CN115322612 A CN 115322612A CN 202211269719 A CN202211269719 A CN 202211269719A CN 115322612 A CN115322612 A CN 115322612A
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- Prior art keywords
- inorganic filler
- hydrophobic
- parts
- dispersion liquid
- super
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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- 239000011256 inorganic filler Substances 0.000 title claims abstract description 116
- 229910003475 inorganic filler Inorganic materials 0.000 title claims abstract description 116
- 238000000576 coating method Methods 0.000 title claims abstract description 58
- 239000011248 coating agent Substances 0.000 title claims abstract description 53
- 239000006185 dispersion Substances 0.000 title claims abstract description 52
- 230000003075 superhydrophobic effect Effects 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 35
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 29
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 18
- 239000002904 solvent Substances 0.000 claims abstract description 18
- -1 polydimethylsiloxane Polymers 0.000 claims abstract description 15
- 239000003960 organic solvent Substances 0.000 claims abstract description 14
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 13
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 13
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 238000007789 sealing Methods 0.000 claims abstract description 12
- 230000004048 modification Effects 0.000 claims abstract description 11
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- 238000000227 grinding Methods 0.000 claims abstract description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 32
- 239000003973 paint Substances 0.000 claims description 23
- 238000003756 stirring Methods 0.000 claims description 18
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 14
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 14
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- 235000012239 silicon dioxide Nutrition 0.000 claims description 9
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 8
- 239000002318 adhesion promoter Substances 0.000 claims description 8
- 239000002270 dispersing agent Substances 0.000 claims description 8
- 239000000080 wetting agent Substances 0.000 claims description 8
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 7
- 229910021485 fumed silica Inorganic materials 0.000 claims description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
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- BPCXHCSZMTWUBW-UHFFFAOYSA-N triethoxy(1,1,2,2,3,3,4,4,5,5,8,8,8-tridecafluorooctyl)silane Chemical compound CCO[Si](OCC)(OCC)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)CCC(F)(F)F BPCXHCSZMTWUBW-UHFFFAOYSA-N 0.000 claims description 6
- 229960000892 attapulgite Drugs 0.000 claims description 5
- 229910052625 palygorskite Inorganic materials 0.000 claims description 5
- 238000007670 refining Methods 0.000 claims description 5
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 4
- 238000009835 boiling Methods 0.000 claims description 4
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 4
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- HXOGQBSDPSMHJK-UHFFFAOYSA-N triethoxy(6-methylheptyl)silane Chemical compound CCO[Si](OCC)(OCC)CCCCCC(C)C HXOGQBSDPSMHJK-UHFFFAOYSA-N 0.000 claims description 4
- 239000011787 zinc oxide Substances 0.000 claims description 4
- 229920002121 Hydroxyl-terminated polybutadiene Polymers 0.000 claims description 3
- ISKQADXMHQSTHK-UHFFFAOYSA-N [4-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=C(CN)C=C1 ISKQADXMHQSTHK-UHFFFAOYSA-N 0.000 claims description 3
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- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 claims description 3
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 2
- ARGICNMLPHJXTP-UHFFFAOYSA-N [SiH4].C(=C)C(OC(CCC)=NO)C(COC(CCC)=O)OC(CCC)=O Chemical compound [SiH4].C(=C)C(OC(CCC)=NO)C(COC(CCC)=O)OC(CCC)=O ARGICNMLPHJXTP-UHFFFAOYSA-N 0.000 claims description 2
- ONNSHOGPJFYSSP-UHFFFAOYSA-N [SiH4].C1(=CC=CC=C1)C(OC(CCC)=NO)C(COC(CCC)=O)OC(CCC)=O Chemical compound [SiH4].C1(=CC=CC=C1)C(OC(CCC)=NO)C(COC(CCC)=O)OC(CCC)=O ONNSHOGPJFYSSP-UHFFFAOYSA-N 0.000 claims description 2
- OUGKFJZADGTJRG-UHFFFAOYSA-N [SiH4].CC(OC(CCC)=NO)C(COC(CCC)=O)OC(CCC)=O Chemical compound [SiH4].CC(OC(CCC)=NO)C(COC(CCC)=O)OC(CCC)=O OUGKFJZADGTJRG-UHFFFAOYSA-N 0.000 claims description 2
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- XGZGKDQVCBHSGI-UHFFFAOYSA-N butyl(triethoxy)silane Chemical compound CCCC[Si](OCC)(OCC)OCC XGZGKDQVCBHSGI-UHFFFAOYSA-N 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims description 2
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- 238000010438 heat treatment Methods 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 5
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 238000005096 rolling process Methods 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical compound CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
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- 229910052751 metal Inorganic materials 0.000 description 3
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- 229910000077 silane Inorganic materials 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 239000008096 xylene Substances 0.000 description 3
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 2
- MTEZSDOQASFMDI-UHFFFAOYSA-N 1-trimethoxysilylpropan-1-ol Chemical compound CCC(O)[Si](OC)(OC)OC MTEZSDOQASFMDI-UHFFFAOYSA-N 0.000 description 2
- VTDQEFPUJUZPCC-UHFFFAOYSA-N N-butan-2-ylidenehydroxylamine silane Chemical compound [SiH4].CCC(C)=NO VTDQEFPUJUZPCC-UHFFFAOYSA-N 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 2
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- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 2
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Classifications
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- C—CHEMISTRY; METALLURGY
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- C09D183/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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- C09C3/12—Treatment with organosilicon compounds
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- C09D183/06—Polysiloxanes containing silicon bound to oxygen-containing groups
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- C09D5/1662—Synthetic film-forming substance
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
本发明属于无机填料和超疏水涂料技术领域，具体涉及一种无机填料分散液、超疏水绝缘耐磨涂料及制备方法。该无机填料分散液首先由疏水硅烷偶联剂对纳米和亚微米无机填料的混合物进行一次改性，再将经一次改性的微纳无机填料与疏水端羟基封闭剂和催化剂于有机溶剂中反应，得到二次改性的无机填料分散液。将该二次改性的无机填料分散液与羟基封端聚二甲基硅氧烷等成分研磨后得到涂料前炼浆，作为增强组分与潜伏型固化剂等成分和溶剂混合均匀，得到单组份超疏水绝缘耐磨涂料。利用该二次改性的无机填料分散液制得的涂料具有优异的超疏水性、绝缘性和耐磨性，在打磨后依然具有优异的超疏水性。
Description
技术领域
本发明涉及无机填料和超疏水绝缘耐磨涂料技术领域，具体涉及一种无机填料分散液、超疏水绝缘耐磨涂料及制备方法。
背景技术
近年来，特高压、高压输电线路建设在电网发展、能源输送和带动经济发展等方面具有重要意义，输变电设备的正常运行更是维护电力系统安全稳定的重要前提。然而，输变电设备长期暴露在复杂多变的自然环境中，使得各类安全事故频发。例如，工业污秽、大气尘埃、鸟类粪便等污染物在绝缘子表面附着极易引发污闪事故；冻雨在输电线路、铁塔表面凝固则容易导致输电线路断路、铁塔倒塌等问题。
为解决以上问题，其中非常有效的方法之一是提高输变电设备表面的疏水性，使得输变电设备不易受到外界污染。例如，使输变电设备的表面形成超疏水表面。超疏水表面是指水接触角大于150°，滚动角小于10°的表面。当水滴在超疏水表面时可快速滚动滑落，同时将超疏水表面的各类污染物冲刷洗脱，提升超疏水表面的清洁度。包括冻雨、冰等物质也很难稳定附着于超疏水表面，其在重力作用下极易从超疏水表面滑落。
对于输变电设备而言，在其表面不仅要形成超疏水表面，而且要求材料的绝缘性以及耐磨性或耐腐蚀性优良。而现有市售的疏水材料，很难满足输变电设备的要求。
发明内容
鉴于此，本发明实施例的目的在于提供一种无机填料分散液、超疏水绝缘耐磨涂料及制备方法，将亚微米无机填料和纳米无机填料的混合物经过二次改性得到无机填料分散液，将此分散液作为增强组分加入涂料中，得到的涂料具有优异的超疏水性、绝缘性和耐磨性。
为达到上述发明目的，本发明实施例第一方面提供了一种无机填料分散液，其包括由纳米无机填料和亚微米无机填料混合而成的微纳无机填料；所述纳米无机填料包括二氧化硅、二氧化钛、氧化锌、硅藻土或凹凸棒土中的至少一种或几种，所述亚微米无机填料包括二氧化硅、二氧化钛、氧化锌、硅藻土或凹凸棒土中的至少一种或几种；其中，所述微纳无机填料依次经疏水硅烷偶联剂一次改性，以及在有机溶剂中经疏水端羟基封闭剂二次改性，形成无机填料分散液；所述有机溶剂为高沸点溶剂和低沸点溶剂的混合，其中，所述高沸点溶剂的沸点为120℃~250℃，所述低沸点溶剂的沸点为70℃~110℃。
对无机填料进行疏水改性的方法在现有技术已有报道，但经实验验证后发现，一方面，改性后的无机填料并非适用于所有涂料体系，在不同涂料体系中所能产生的疏水效果并不相同，例如适用于树脂体系并能使涂层具备疏水性的改性无机填料在应用于有机硅涂料体系时，存在疏水性能下降的情况；另一方面，含有改性疏水填料的涂料实际上并不都能同时兼具良好的超疏水性和耐磨性。
本发明利用疏水硅烷偶联剂和疏水端羟基封闭剂改性微纳无机填料，疏水硅烷偶联剂可赋予微纳无机填料低表面能，降低其发生自团聚的机率；同时还可提升其与涂料体系的不相容性，使制得的无机填料分散液中二次改性的无机填料在涂层体相和界面处富集，进而使涂层表面形成超疏水微纳结构。利用疏水端羟基封闭剂对经一次改性的微纳无机填料进行二次改性，一方面可以提升所得二次改性的无机填料的疏水性，另一方面其还可以与后续制备超疏水涂料过程中使用的固化剂丁酮肟硅烷反应，使经二次改性的无机填料分散液参与固化反应，从而高效固载于涂层表面，形成稳定的超疏水耐磨微纳涂层。
结合第一方面，所述疏水硅烷偶联剂为异辛基三乙氧基硅烷、丁基三乙氧基硅烷、γ -缩水甘油醚氧丙基三甲氧基硅烷或γ -甲基丙烯酰氧基丙基三甲氧基硅烷中的至少一种与十三氟辛基三乙氧基硅烷的组合。其中疏水硅烷偶联剂在弱碱性（例如pH8~10）、60℃~70℃环境中，可用于修饰微纳无机填料的表面。所述疏水端羟基封闭剂为羟基封端聚二甲基硅氧烷、羟基封端聚丁二烯聚氨酯或羟基封端聚丙二醇。
结合第一方面，所述疏水硅烷偶联剂的添加量为所述微纳无机填料总质量的0.5%~3.0%，所述疏水端羟基封闭剂的添加量为经所述一次改性的微纳无机填料总质量的5%~20%。
结合第一方面，所述纳米无机填料粒径为5nm~50nm，所述亚微米无机填料粒径为100nm~500nm；在所述微纳无机填料中，纳米无机填料的质量百分比为25%~50%，亚微米无机填料的质量百分比为50%~75%。不同粒径的亚微米无机填料和纳米无机填料的组合有利于涂料漆膜表面形成具有微纳结构的超疏水表面，进而赋予涂层超疏水性能。
本发明实施例的第二方面，提供上述无机填料分散液的制备方法，其包括以下步骤：
S1、将所述微纳无机填料分散于乙醇中，加入氨水调节体系pH至8~10，再加入疏水硅烷偶联剂，在60℃~70℃搅拌2.5~3.5小时，固液分离，将所得固体干燥，得到一次改性的微纳无机填料；
S2、将所述一次改性的微纳无机填料分散于有机溶剂中，加入疏水端羟基封闭剂和催化剂，在115℃~125℃搅拌2.5~3.5小时，得到二次改性的无机填料分散液；其中，所述催化剂为二月桂酸二丁基锡、辛酸亚锡、二醋酸二丁基锡中的一种。
该无机填料分散液为经过二次改性的三重修饰的无机填料分散液，具有良好的超疏水性和绝缘性。将该无机填料分散液作为增强组分可用于与有机硅树脂、其他颜填料、涂料助剂和有机溶剂按涂料的常规制备方法进行制备，即可得到单组份超疏水绝缘耐磨涂料。本发明实施例的制备方法简单、能够对微纳无机填料进行充分改性。
结合本发明第二方面，所述有机溶剂的添加量为所述一次改性的微纳无机填料总质量的5~7倍。
选用高沸点有机溶剂和低沸点有机溶剂组合构成无机填料分散液溶剂体系，在后续制备涂料过程中，低沸点有机溶剂挥发速度快，有利于涂层体相中二次改性的无机填料向涂层表面迁移；而高沸点有机溶剂挥发速度慢，有利于减缓涂料的成膜速度，延长二次改性的无机填料向涂层表面迁移的时间，进而使涂层表面含有大量二次改性的无机填料，增强涂层超疏水性能。
第三方面，本发明实施例提供一种超疏水绝缘耐磨涂料，包括以下质量配比的组分：
上述的无机填料分散液350~360份，无机填料分散液中固含量为10%~20%，
羟基封端聚二甲基硅氧烷55~70份，
碳酸钙45~60份，
硫酸钡15~35份，
气相二氧化硅10~15份，
消泡剂0.4~0.7份，
分散剂1.5~2.5份，
潜伏型固化剂40~50份，
基材润湿剂0.8~1.5份，
附着力促进剂2~3份，和
溶剂10~15份。
本发明第四方面，还提供了上述超疏水绝缘耐磨涂料的制备方法，其包括以下步骤：
S1、将设计量的所述羟基封端聚二甲基硅氧烷、碳酸钙、硫酸钡、气相二氧化硅、消泡剂、分散剂加入所述无机填料分散液中，搅拌分散均匀，研磨得到涂料前炼浆；
S2、将所述潜伏型固化剂、基材润湿剂、附着力促进剂、溶剂加入所述涂料前炼浆中，搅拌分散均匀，得到超疏水绝缘耐磨涂料。
结合第四方面，S1中所述涂料前炼浆的平均粒径不大于25微米；
S2中所述潜伏型固化剂为乙烯基三丁酮肟基硅烷、甲基三丁酮肟基硅烷或苯基三丁酮肟基硅烷。丁酮肟硅烷与羟基封端聚二甲基硅氧烷组成单组份涂料基体树脂体系，二者在空气中的水汽作用下可以迅速交联固化，提高了涂膜的表面附着力。
本发明实施例中，将所得无机填料分散液经与羟基封端聚二甲基硅氧烷等成分研磨后可作为增强组分，与潜伏型固化剂等成分和溶剂混合后，可制得单组份超疏水绝缘耐磨涂料。本发明提供的利用二次改性的无机填料分散液制得的超疏水绝缘耐磨涂料体系属于有机硅体系，其涂层具有优异的超疏水性、绝缘性和耐磨性，水接触角大于155°，滚动角小于5°，体积电阻率大于1.0×1012Ω·m，且在打磨后依然具有优异的超疏水性，可广泛应用于玻璃、陶瓷、金属基材等领域，尤其是高压设备等领域，在输变电设备的表面涂覆本发明实施例中涂料，在设备表面形成超疏水的结构，冻雨、冰等物质也很难稳定附着于超疏水表面，其在重力作用下极易从超疏水表面滑落，很大程度上减少相关事故的发生。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白，下面对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅用以解释本发明，并不用于限定本发明。
以下实施例中所用消泡剂型号为Tego Airex 931，分散剂型号为Tego Dispers650，附着力促进剂选用三众友SY 5620，基材润湿剂型号为Tego270。
实施例1
本实施例提供的无机填料分散液，其制备方法为：
（1）将35份（重量份，下同）纳米二氧化硅（平均粒径10nm）、65份亚微米二氧化钛（平均粒径250nm）加入1000份乙醇中，开启电动搅拌，再加入浓氨水调节体系pH至8.5，依次加入1.8份十三氟辛基三乙氧基硅烷和1.2份异辛基三乙氧基硅烷，升温至60℃，反应3小时，将体系在6000 转/分钟条件下离心30分钟，收集沉淀，并在105℃烘箱中干燥5小时，得到一次改性的微纳无机填料；
（2）将180份二甲苯、120份二氯乙烷、50份一次改性的微纳无机填料、4.0份羟基封端聚二甲基硅氧烷和0.1份二月桂酸二丁基锡置于反应釜中，搅拌均匀后升温至120℃反应3小时，制得二次改性的无机填料分散液。
实施例2
本实施例提供的无机填料分散液，其制备方法为：
（1）将32份纳米二氧化硅（平均粒径10nm）、68份亚微米硅藻土（平均粒径400nm）加入1000份乙醇中，开启电动搅拌，再加入浓氨水调节体系pH至8.8，依次加入1.4份十三氟辛基三乙氧基硅烷和0.7份γ -缩水甘油醚氧丙基三甲氧基硅烷，升温至65℃，反应3小时，将体系在6000 转/分钟条件下离心30分钟，收集沉淀，并在105℃烘箱中干燥5小时，得到一次改性的微纳无机填料；
（2）将150份200号溶剂油、150份二氧六环、50 份一次改性的微纳无机填料、6.2份羟基封端聚丁二烯聚氨酯和0.1份辛酸亚锡置于反应釜中，搅拌均匀后升温至120℃反应3小时，制得二次改性的无机填料分散液。
实施例3
本实施例提供的无机填料分散液，其制备方法为：
（1）将37份纳米二氧化硅（平均粒径25nm）、63份亚微米凹凸棒土（平均粒径350nm）加入1000份乙醇中，开启电动搅拌，再加入浓氨水调节体系pH至9.0，依次加入1.9份十三氟辛基三乙氧基硅烷和1.0份异辛基三乙氧基硅烷，升温至60℃，反应3小时，将体系在6000转/分钟条件下离心30分钟，收集沉淀，并在105℃烘箱中干燥5小时，得到一次改性的微纳无机填料；
（2）将166份异链烷烃、134份二氯乙烷、50份一次改性的微纳无机填料、5.0份羟基封端聚丙二醇和0.1份二醋酸二丁基锡置于反应釜中，搅拌均匀后升温至120℃反应3小时，制得二次改性的疏水无机填料分散液。
实施例4
本实施例提供一种超疏水绝缘耐磨涂料，其制备方法为：
（1）将实施例1得到的无机填料分散液358份、60份羟基封端聚二甲基硅氧烷、55份碳酸钙、20份硫酸钡、15份气相二氧化硅、0.6份有机硅消泡剂和2.0份分散剂依次混合，搅拌分散均匀后，用卧式砂磨将分散体系研磨至细度小于25微米，并转移至密封调漆罐中；
（2）将调漆罐抽真空，充氮气，重复三次，再向调漆罐中依次加入45份乙烯基三丁酮肟基硅烷、1.0份基材润湿剂、2.5份附着力促进剂、13份铁红色浆和10份二甲苯，搅拌均匀后，出料，密封保存，制得单组份超疏水绝缘耐磨涂料。
实施例5
本实施例提供一种超疏水绝缘耐磨涂料，其制备方法为：
（1）将实施例2得到的无机填料分散液355份、70份羟基封端聚二甲基硅氧烷、50份碳酸钙、18份硫酸钡、12份气相二氧化硅、0.5份消泡剂和1.8 份分散剂依次混合，搅拌分散均匀后，用卧式砂磨将分散体系研磨至细度小于25微米，并转移至密封调漆罐中；
（2）将调漆罐抽真空，充氮气，重复三次，再向调漆罐中依次加入47份乙烯基三丁酮肟基硅烷、1.0份基材润湿剂、2.5份附着力促进剂、13份铁红色浆和12份200号溶剂油，搅拌均匀后，出料，密封保存，制得单组份超疏水绝缘涂料。
实施例6
本实施例提供一种超疏水绝缘耐磨涂料，其制备方法为：
（1）将实施例3得到的无机填料分散液355份、55份羟基封端聚二甲基硅氧烷、50份碳酸钙、34份硫酸钡、11份气相二氧化硅、0.6份消泡剂和1.9份分散剂依次混合，搅拌分散均匀后，用卧式砂磨将分散体系研磨至细度小于25微米，并转移至密封调漆罐中；
（2）将调漆罐抽真空，充氮气，重复三次，再向调漆罐中依次加入44份甲基三丁酮肟基硅烷、1.0份基材润湿剂、2.5份附着力促进剂、13份铁红色浆、10份异链烷烃，搅拌均匀后，出料，密封保存，制得单组份超疏水绝缘涂料。
对比例1
将100份纳米二氧化硅加入1000份乙醇中，开启电动搅拌，再加入浓氨水调节体系pH至8.8，依次加入1.4份十三氟辛基三乙氧基硅烷和0.7份γ -缩水甘油醚氧丙基三甲氧基硅烷，升温至65℃，反应3小时，将体系在6000 转/分钟条件下离心30分钟，收集沉淀，并在105℃烘箱中干燥5小时，得到一次改性的微纳无机填料；其余步骤依次同实施例1和实施例4。
对比例2
参照对比例1制备超疏水绝缘耐磨涂料，将制备过程中的纳米二氧化硅替换为亚微米二氧化钛，其余步骤与对比例1相同。
对比例3
参照实施例1制备一次改性的微纳无机填料，并将50份一次改性的微纳无机填料、300份二甲苯、4.0份羟基封端聚二甲基硅氧烷和0.1份二月桂酸二丁基锡置于反应釜中，搅拌均匀后升温至120℃反应3小时，制得二次改性的无机填料分散液；其余步骤同实施例4。
对比例4
参照对比例3制备超疏水绝缘耐磨涂料，将对比例3中用到的二甲苯替换为二氯乙烷，其余步骤同对比例3剩余步骤。
对比例5
参照实施例2中步骤（1）制备得到一次改性的微纳无机填料，并将50 份一次改性的微纳无机填料分散在150份200号溶剂油、150份二氧六环中，其余步骤参照实施例4制备超疏水绝缘耐磨涂料。
检验
将实施例4~6和对比例1~5所制备的涂料涂覆于玻璃表面，室温固化7天后，所得漆膜附着力、水接触角、滚动角、体积电阻率以及打磨后的水接触角和滚动角数据见表1（打磨条件为用800目砂纸在500 kPa压力下打磨100次）。
需要说明的是，本发明实施例中的涂料还可用于陶瓷表面、金属基材表面等。上述实验中的玻璃表面只是其中一种应用场景。当将实施例4~6和对比例1~5所制备的涂料涂覆在金属基材或陶瓷表面时，具有与玻璃表面相似的性能和效果；例如涂在高压裸线上时，可实现超疏水的表面。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。
Claims (9)
1.一种无机填料分散液，其特征在于，包括由纳米无机填料和亚微米无机填料混合而成的微纳无机填料；所述纳米无机填料包括二氧化硅、二氧化钛、氧化锌、硅藻土或凹凸棒土中的至少一种或几种，所述亚微米无机填料包括二氧化硅、二氧化钛、氧化锌、硅藻土或凹凸棒土中的至少一种或几种；
其中，所述微纳无机填料依次经疏水硅烷偶联剂一次改性，以及在有机溶剂中经疏水端羟基封闭剂二次改性，形成无机填料分散液；所述有机溶剂为高沸点溶剂和低沸点溶剂的混合，其中，所述高沸点溶剂的沸点为120℃~250℃，所述低沸点溶剂的沸点为70℃~110℃。
2.如权利要求1所述的无机填料分散液，其特征在于，所述疏水硅烷偶联剂为异辛基三乙氧基硅烷、丁基三乙氧基硅烷、γ -缩水甘油醚氧丙基三甲氧基硅烷或γ -甲基丙烯酰氧基丙基三甲氧基硅烷中的至少一种与十三氟辛基三乙氧基硅烷的组合；
所述疏水端羟基封闭剂为羟基封端聚二甲基硅氧烷、羟基封端聚丁二烯聚氨酯或羟基封端聚丙二醇。
3.如权利要求1或2所述的无机填料分散液，其特征在于，所述疏水硅烷偶联剂的添加量为所述微纳无机填料总质量的0.5%~3.0%；
所述疏水端羟基封闭剂的添加量为经所述一次改性的微纳无机填料总质量的5%~20%。
4.如权利要求1所述的无机填料分散液，其特征在于，所述纳米无机填料粒径为5nm~50nm，所述亚微米无机填料粒径为100nm~500nm；
在所述微纳无机填料中，纳米无机填料的质量百分比为25%~50%，亚微米无机填料的质量百分比为50%~75%。
5.一种无机填料分散液的制备方法，其特征在于，所述制备方法用于制备权利要求1~4任一项所述的无机填料分散液，包括以下步骤：
S1、将所述微纳无机填料分散于乙醇中，加入氨水调节体系pH至8~10，再加入疏水硅烷偶联剂，在60℃~70℃搅拌2.5~3.5小时，固液分离，将所得固体干燥，得到一次改性的微纳无机填料；
S2、将所述一次改性的微纳无机填料分散于有机溶剂中，加入疏水端羟基封闭剂和催化剂，在115℃~125℃搅拌2.5~3.5小时，得到二次改性的无机填料分散液；
其中，所述催化剂为二月桂酸二丁基锡、辛酸亚锡或二醋酸二丁基锡中的一种。
6.如权利要求5所述无机填料分散液的制备方法，其特征在于，所述有机溶剂的添加量为所述一次改性的微纳无机填料总质量的5~7倍。
7.一种超疏水绝缘耐磨涂料，其特征在于，包括以下质量配比的组分：
权利要求1~4任一项所述的无机填料分散液或权利要求5~6任一项所述制备方法制得的无机填料分散液350~360份，无机填料分散液中固含量为10%~20%，
羟基封端聚二甲基硅氧烷55~70份，
碳酸钙45~60份，
硫酸钡15~35份，
气相二氧化硅10~15份，
消泡剂0.4~0.7份，
分散剂1.5~2.5份，
潜伏型固化剂40~50份，
基材润湿剂0.8~1.5份，
附着力促进剂2~3份，和
溶剂10~15份。
8.一种超疏水绝缘耐磨涂料的制备方法，其特征在于，所述制备方法用于制备权利要求7所述的超疏水绝缘耐磨涂料，包括以下步骤：
S1、称取设计量的所述羟基封端聚二甲基硅氧烷、碳酸钙、硫酸钡、气相二氧化硅、消泡剂和分散剂加入所述无机填料分散液中，搅拌分散均匀，研磨得到涂料前炼浆；
S2、将所述潜伏型固化剂、基材润湿剂、附着力促进剂、溶剂加入所述涂料前炼浆中，搅拌分散均匀，得到超疏水绝缘耐磨涂料。
9.如权利要求8所述超疏水绝缘耐磨涂料的制备方法，其特征在于，
S1中所述涂料前炼浆的平均粒径不大于25微米；
S2中所述潜伏型固化剂为乙烯基三丁酮肟基硅烷、甲基三丁酮肟基硅烷或苯基三丁酮肟基硅烷。
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