WO2018108015A1 - 一种石墨烯改性无机涂料及其制备方法 - Google Patents

一种石墨烯改性无机涂料及其制备方法 Download PDF

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WO2018108015A1
WO2018108015A1 PCT/CN2017/114903 CN2017114903W WO2018108015A1 WO 2018108015 A1 WO2018108015 A1 WO 2018108015A1 CN 2017114903 W CN2017114903 W CN 2017114903W WO 2018108015 A1 WO2018108015 A1 WO 2018108015A1
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graphene
parts
inorganic coating
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吕维忠
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Shenzhen University
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic

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  • the invention relates to the field of coatings, in particular to a graphene-modified inorganic coating and a preparation method thereof.
  • Glass insulation inorganic coatings are mainly composed of inorganic nano ceramic resin, polyurethane resin, silicone resin, nano indium tin oxide (ITO) powder, nano tin oxide antimony (ATO) powder, coating additives and thinner. .
  • the coating has the advantages of good heat insulation effect, excellent light transmission performance, aging resistance and radiation protection.
  • the object of the present invention is to provide a graphene-modified inorganic coating, which aims to solve the problems of low hardness, poor adhesion and low abrasion resistance of the prior inorganic coatings applied to the surface of glass. The problem.
  • a graphene-modified inorganic coating comprising graphene and an inorganic coating, the graphene accounting for 0.001% to 5% by weight of the inorganic coating.
  • the graphene-modified inorganic coating material comprises, in mass percentage, the inorganic coating material comprises: 50 to 90 parts of a high hardness polymer resin, 10 to 50 parts of a nano heat insulation slurry, and a cosolvent agent. ⁇ 10 parts, 0 to 0.5 parts of antifoaming agent, 0 to 0.5 parts of suds suppressor, 0 to 0.5 parts of substrate wetting agent, and 0 to 0.5 parts of leveling agent.
  • the graphene-modified electrodeless coating wherein the graphene comprises carbon elements and non-carbon elements, and the non-carbon elements are fluorine, nitrogen, oxygen, sulfur, hydrogen, chlorine, bromine, and iodine.
  • the non-carbon elements are fluorine, nitrogen, oxygen, sulfur, hydrogen, chlorine, bromine, and iodine.
  • the graphene-modified inorganic coating material has a mass ratio of carbon element to non-carbon element in the graphene of 4 to 6:1.
  • the graphene-modified inorganic coating material wherein the graphene is a single-layer sheet structure.
  • the graphene-modified inorganic coating material wherein the graphene is a combined sheet structure of 2 to 50 layers, the inter-layer carbon atoms are bonded by a ⁇ bond, and the carbon atoms in the layer are composed of sp 2 hybrid orbitals. Hexagonal honeycomb lattice.
  • the graphene-modified inorganic coating material wherein the graphene is a modified graphene with a functional group modification, the functional group is one or more of a hydroxyl group, a carboxyl group, a nitrogen group, and an amino group. .
  • the graphene-modified inorganic coating material wherein the graphene is in the form of a powder or a slurry.
  • the graphene-modified inorganic coating material, wherein the nano-insulation slurry is one of ITO, ATO or a mixture thereof.
  • a method for preparing a graphene modified electrodeless coating comprising the steps of:
  • the present invention provides a graphene-modified inorganic coating composition comprising graphene and an inorganic coating, and the method for preparing the same, wherein the graphene accounts for 0.001% by weight of the inorganic coating. ⁇ 5%.
  • the adhesion and hardness of the graphene-modified inorganic coating prepared by the invention are greatly improved compared with the common inorganic coatings, and the coating film has good adhesion and better resistance when applied to the glass surface by using the coating of the invention. Abrasiveness, while reducing energy consumption and increasing the conductivity of the coating.
  • FIG. 1 is a flow chart of a preferred embodiment of a method for preparing a graphene-modified inorganic coating according to the present invention.
  • the present invention provides a graphene-modified inorganic coating material, and the present invention will be further described in detail below in order to clarify and clarify the objects, technical solutions and effects of the present invention. It should be understood that the specifics described herein The examples are merely illustrative of the invention and are not intended to limit the invention.
  • the present invention provides a graphene-modified inorganic coating comprising graphene and an inorganic coating, which accounts for 0.001% to 5% by mass of the inorganic coating.
  • graphene is currently the thinnest but hardest nanomaterial in the world. It is almost completely transparent and has a thermal conductivity of up to 5300 W/m.k, which is higher than that of carbon nanotubes and diamond.
  • Graphene is a new material of a single-layer sheet structure composed of carbon atoms, and has the characteristics of high strength, large specific surface area, high chemical reactivity, and high filling property.
  • graphene has the characteristics of softness, planar structure and high strength, when it is uniformly dispersed in inorganic matter, the planar structure of graphene can improve the adsorption capacity, and the flexibility of graphene can inhibit the inorganic matter under the action of drying and external heating field.
  • the shrinkage property, thereby suppressing cracking, and the high strength property of graphene in the planar direction can increase the overall strength of the inorganic film after film formation. Therefore, the addition of graphene to the inorganic coating can make the coating more tightly contact with the substrate, and at the same time, because of the good lubricating effect of the graphene, the adhesion and the abrasion resistance of the coating on the glass surface can be improved.
  • controlling the amount of graphene added is extremely critical, and if the amount of graphene added is less than 0.001% of the amount of the inorganic coating, the inorganic coating cannot be improved on the glass surface.
  • the amount of the graphene added is 0.1% to 1% by mass of the inorganic coating, and within this range, the modification effect of the inorganic coating is optimal.
  • the inorganic coating material comprises, by mass percentage, 50 to 90 parts of a high hardness polymer resin, 10 to 50 parts of a nano heat insulation slurry, 0 to 10 parts of a cosolvent, and an antifoaming agent 0 to 0.5 parts, 0 to 0.5 parts of the suds suppressor, 0 to 0.5 parts of the substrate wetting agent, and 0 to 0.5 parts of the leveling agent;
  • the high hardness polymer resin is an inorganic ceramic resin
  • the nano heat insulating paste The material is one of ITO, ATO or a mixture thereof.
  • the graphene includes a carbon element and a non-carbon element, and the non-carbon element is one or more of fluorine, nitrogen, oxygen, sulfur, hydrogen, chlorine, bromine, and iodine;
  • the mass ratio of carbon to non-carbon in graphene is 4-6:1.
  • controlling the mass ratio of carbon elements to non-carbon elements in graphene At 5:1, at this ratio, it is ensured that graphene can improve the adhesion of the inorganic coating on the glass surface and the friction resistance.
  • the graphene is in the form of a powder or a slurry, and is sufficiently mixed with the inorganic coating during the preparation to exert an effect of enhancing the adhesion and abrasion resistance of the coating on the glass surface.
  • the graphene is a single-layer sheet structure having a unique two-dimensional structure and excellent mechanical, thermodynamic, optical and electrical properties.
  • the graphene may also be a combined sheet structure of 2 to 50 layers, the inter-layer carbon atoms are bonded by a ⁇ bond, and the carbon atoms in the layer are formed into a hexagonal honeycomb lattice by a sp 2 hybrid orbital.
  • the graphene used in the present invention is a modified graphene having a functional group modified, and the functional group is one or more of a hydroxyl group, a carboxyl group, a nitrogen group, and an amino group, and the modified graphene can further improve the graphene. Its own adsorption capacity, thereby improving the adsorption capacity of graphene modified inorganic coatings.
  • the present invention also provides a method for preparing a graphene modified electrodeless coating, as shown in FIG. 1 , wherein the method comprises the following steps:
  • Comparative Example 1 a commercially available conventional glass-insulating inorganic coating.
  • Comparative Example 2 the formulation and preparation method were the same as in Example 1, except that high hardness graphene was not added.
  • the present invention uses high hardness graphene to modify the existing glass heat insulating inorganic coating, which can greatly improve the adhesion of the coating on the glass surface, and at the same time, the hardness of the coating can be improved due to the good lubricating effect of the graphene. And abrasion resistance.
  • the present invention provides a graphene-modified inorganic coating comprising graphene and an inorganic coating, and the method for preparing the same, wherein the graphene accounts for inorganic coatings by mass percentage. 0.001% to 5%.
  • the adhesion and hardness of the graphene-modified inorganic coating prepared by the invention are greatly improved compared with the common inorganic coatings, and the coating film has good adhesion and better resistance when applied to the glass surface by using the coating of the invention. Abrasiveness, while reducing energy consumption and increasing the conductivity of the coating.

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
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Abstract

一种石墨烯改性无机涂料及其制备方法，该涂料包括石墨烯和无机涂料，按质量百分比计，石墨烯占无机涂料的0.001%~5%。制备方法是先添加一定量的高硬度聚合物树脂和纳米隔热浆料，再依次加入助熔剂、消泡剂、抑泡剂、基材润湿剂和流平剂，混合均匀，最后加入石墨烯，搅拌得到该涂料。

Description

一种石墨烯改性无机涂料及其制备方法 技术领域
本发明涉及涂料领域，尤其涉及的是一种石墨烯改性无机涂料及其制备方法。
背景技术
二十世纪以来世界能源消耗大幅度增加，节能降耗，提高经济效益是科学研究和技术开发的主要目标，开发隔热保温的环保材料具有极其重要的意义。玻璃隔热无机涂料能充分解决建筑门窗的隔热保温问题，不仅节约了能源，还能为人们营造冬暖夏凉、舒适宜居的室内环境。
玻璃隔热无机涂料主要是由无机纳米陶瓷树脂、聚氨酯树脂、聚硅氧烷树脂、纳米氧化铟锡(ITO)粉体、纳米氧化锡锑(ATO)粉体，涂料助剂和稀释剂等组成。该涂料具有隔热效果良好、透光性能优异、耐老化及防辐射等优点。
然而，采用无机涂料涂覆于玻璃材料时，存在附着力差、耐摩擦性较低等问题。
因此，现有技术还有待于改进和发展。
发明内容
鉴于上述现有技术的不足，本发明的目的在于提供一种石墨烯改性无机涂料，旨在解决现有无机涂料涂覆于玻璃表面时存在的硬度低、附着力差以及耐摩擦性较低的问题。
本发明的技术方案如下：
一种石墨烯改性无机涂料，其中，包括石墨烯和无机涂料，按质量百分比计，所述石墨烯占无机涂料的0.001％～5％。
较佳地，所述的石墨烯改性无机涂料，其中，按质量百分比计，所述无机涂料包括：高硬度聚合物树脂50～90份、纳米隔热浆料10～50份、助溶剂0～10份、消泡剂0～0.5份、抑泡剂0～0.5份、基材润湿剂0～0.5份以及流平剂0～0.5份。
较佳地，所述的石墨烯改性无极涂料，其中，所述石墨烯包括碳元素和非碳元素，所述非碳元素为氟、氮、氧、硫、氢、氯、溴、碘中的一种或几种。
较佳地，所述的石墨烯改性无机涂料，其中，所述石墨烯中，碳元素与非碳元素的质量比为4～6:1。
较佳地，所述的石墨烯改性无机涂料，其中，所述石墨烯为单层片状结构。
较佳地，所述的石墨烯改性无机涂料，其中，所述石墨烯为2～50层组合片状结构，层间碳原子以π键结合，层内碳原子以sp2杂化轨道组成六角形蜂巢状晶格。
较佳地，所述的石墨烯改性无机涂料，其中，所述石墨烯为带有官能团修饰的改性石墨烯，所述官能团为羟基、羧基、氮基、氨基中的一种或几种。
较佳地，所述的石墨烯改性无机涂料，其中，所述石墨烯为粉末状或浆料状。
较佳地，所述的石墨烯改性无机涂料，其中，所述纳米隔热浆料为ITO、ATO中的一种或其混合物。
一种石墨烯改性无极涂料的制备方法，其中，包括步骤：
按质量百分比计，先将50～90份的高硬度聚合物树脂和10～50份的纳米隔热浆料混合均匀，再依次加入0～10份的助溶剂、0～0.5份的消泡剂、0～0.5份的抑泡剂、0～0.5份的基材润湿剂以及0～0.5份的流平剂混合均匀；
最后加入0.001～5份的石墨烯，在500-700r/min的搅拌速度下搅拌30-80min后，得到石墨烯改性无机涂料。
有益效果：本发明提供一种石墨烯改性无机涂料及其制备方法，所述石墨烯改性无机涂料由石墨烯和无机涂料组成，按质量百分比计，所述石墨烯占无机涂料的0.001％～5％。本发明制备的石墨烯改性无机涂料的附着力、硬度较普通的无机涂料有了较大的提高，使用本发明涂料涂覆于玻璃表面时，涂膜具有良好的附着力和更好的耐磨性，同时降低了能耗，提高了涂层的导电率。
附图说明
图1为本发明一种石墨烯改性无机涂料制备方法较佳实施例的流程图。
具体实施方式
本发明提供一种石墨烯改性无机涂料，为使本发明的目的、技术方案及效果更加清楚、明确，以下对本发明进一步详细说明。应当理解，此处所描述的具体 实施例仅仅用以解释本发明，并不用于限定本发明。
本发明提供一种石墨烯改性无机涂料，其中，包括石墨烯和无机涂料，按质量百分比计，所述石墨烯占无机涂料的0.001％～5％。
具体地，石墨烯是目前世界上最薄却是最坚硬的纳米材料，它几乎是完全透明的，其导热系数高达5300W/m.k，高于碳纳米管和金刚石。石墨烯是一种由碳原子构成的单层片状结构的新材料，具有强度高、比表面积大、高化学反应活性、高填充性的特点。
由于石墨烯具有柔软、平面状结构、强度高等特征，均匀分散在无机物中时，平面状结构的石墨烯可提高吸附能力，石墨烯的柔软性可抑制无机物在干燥及外加热场作用下的收缩性，从而抑制龟裂，石墨烯沿平面方向的高强度特性可增加无机物成膜后的整体强度。因此，在无机涂料中加入石墨烯可使得涂层对底材接触更加紧密，同时由于石墨烯润滑效果好，还能提高涂料在玻璃表面的附着力和耐摩擦性。
进一步，在本发明制备石墨烯改性无机涂料的过程中，控制石墨烯的加入量异常关键，若石墨烯的添加量低于无机涂料用量的0.001％，则无法起到提高无机涂料在玻璃表面上的附着力和耐摩擦性的效果；若果石墨烯的添加量高于无极涂料用量的5％，则会影响无机涂料的成膜性能，降低成膜质量。较佳地，本发明优选所述石墨烯的加入量占无机涂料的质量百分比为0.1％-1％，在该值范围内，无机涂料的改性效果最佳。
进一步，在本发明中，按质量百分比计，所述无机涂料包括：高硬度聚合物树脂50～90份、纳米隔热浆料10～50份、助溶剂0～10份、消泡剂0～0.5份、抑泡剂0～0.5份、基材润湿剂0～0.5份以及流平剂0～0.5份；优选地，所述高硬度聚合物树脂为无机陶瓷树脂，所述纳米隔热浆料为ITO、ATO中的一种或其混合物。
进一步，在本发明中，所述石墨烯包括碳元素和非碳元素，所述非碳元素为氟、氮、氧、硫、氢、氯、溴、碘中的一种或几种；并且所述石墨烯中碳元素与非碳元素的质量比为4～6:1。优选地，控制石墨烯中碳元素与非碳元素的质量比 为5:1，在该比例值时，保证了石墨烯能起到良好的提高无机涂料在玻璃表面附着力和耐摩擦性的改性效果。
进一步，在本发明中，所述石墨烯为粉末状或浆料状，便于在制备过程中与无机涂料充分混合，从而发挥增强涂料在玻璃表面的附着力和耐摩擦性的效果。
更进一步，在本发明中所述石墨烯为单层片状结构，它拥有独特的二维结构和优异的力学、热力学、光学和电学性能。当然所述石墨烯还可以为2～50层组合片状结构，层间碳原子以π键结合，层内碳原子以sp2杂化轨道组成六角形蜂巢状晶格。
进一步，本发明所使用的石墨烯为带有官能团修饰的改性石墨烯，所述官能团为羟基、羧基、氮基、氨基中的一种或几种，改性后的石墨烯可进一步提高其自身的吸附能力，从而提高石墨烯改性无机涂料的吸附能力。
基于上述一种石墨烯改性无机涂料，本发明还提供一种石墨烯改性无极涂料的制备方法，如图1所示，其中，包括步骤：
S100、按质量百分比计，先将50～90份的高硬度聚合物树脂和10～50份的纳米隔热浆料混合均匀，再依次加入0～10份的助溶剂、0～0.5份的消泡剂、0～0.5份的抑泡剂、0～0.5份的基材润湿剂以及0～0.5份的流平剂混合均匀；
S200、最后加入0.001～5份的石墨烯，在500-700r/min的搅拌速度下搅拌30-80min后，得到石墨烯改性无机涂料。
下面通过具体实施例对本发明一种石墨烯改性无极涂料的制备方法进行解释说明：
实施例1
将无机陶瓷树脂50％、ATO浆料40％混合均匀，然后加入助溶剂3％、消泡剂0.5％、抑泡剂0.5％、基材润湿剂0.5％、流平剂0.5％混合均匀，最后加入高硬度石墨烯5％，保持500r/min，分散30min，得石墨烯改性玻璃隔热无机涂料。
实施例2
将无机陶瓷树脂60％、ATO浆料30％混合均匀，然后加入助溶剂7％、消泡剂0.5％、抑泡剂0.5％、基材润湿剂0.5％、流平剂0.5％混合均匀，最后加入高 硬度石墨烯1％，保持700r/min，分散80min，得石墨烯改性玻璃隔热无机涂料。
实施例3
将无机陶瓷树脂70％、ATO浆料20％混合均匀，然后加入助溶剂7.9％、消泡剂0.5％、抑泡剂0.5％、基材润湿剂0.5％、流平剂0.5％混合均匀，，最后加入高硬度石墨烯0.1％，保持600r/min，分散60min，得石墨烯改性玻璃隔热无机涂料。
对比例1，市售传统玻璃隔热无机涂料。
对比例2，所用配方与制法与实施例1相同，区别在于未加入高硬度石墨烯。
将实施例1-3得到的高硬度石墨烯改性玻璃隔热无机涂料与对比例1-2的玻璃隔热无机涂料直接涂覆在玻璃表面，进行对比测试，结果如表1所示：
表1、测试结果
Figure PCTCN2017114903-appb-000001
由表1的结果可见，本发明采用高硬度石墨烯改性现有的玻璃隔热无机涂料，能大大提高涂料在玻璃表面的附着力，同时由于石墨烯润滑效果好，可提高涂层的硬度和耐摩擦性。
综上所述，本发明提供一种石墨烯改性无机涂料及其制备方法，所述石墨烯改性无机涂料包括石墨烯和无机涂料，按质量百分比计，所述石墨烯占无机涂料 的0.001％～5％。本发明制备的石墨烯改性无机涂料的附着力、硬度较普通的无机涂料有了较大的提高，使用本发明涂料涂覆于玻璃表面时，涂膜具有良好的附着力和更好的耐磨性，同时降低了能耗，提高了涂层的导电率。
应当理解的是，本发明的应用不限于上述的举例，对本领域普通技术人员来说，可以根据上述说明加以改进或变换，所有这些改进和变换都应属于本发明所附权利要求的保护范围。

Claims (10)

  1. 一种石墨烯改性无机涂料，其特征在于，包括石墨烯和无机涂料，按质量百分比计，所述石墨烯占无机涂料的0.001％～5％。
  2. 根据权利要求1所述的石墨烯改性无机涂料，其特征在于，按质量百分比计，所述无机涂料包括：高硬度聚合物树脂50～90份、纳米隔热浆料10～50份、助溶剂0～10份、消泡剂0～0.5份、抑泡剂0～0.5份、基材润湿剂0～0.5份以及流平剂0～0.5份。
  3. 根据权利要求1所述的石墨烯改性无极涂料，其特征在于，所述石墨烯包括碳元素和非碳元素，所述非碳元素为氟、氮、氧、硫、氢、氯、溴、碘中的一种或几种。
  4. 根据权利要求3所述的石墨烯改性无机涂料，其特征在于，所述石墨烯中，碳元素与非碳元素的质量比为4～6:1。
  5. 根据权利要求1所述的石墨烯改性无机涂料，其特征在于，所述石墨烯为单层片状结构。
  6. 根据权利要求1所述的石墨烯改性无机涂料，其特征在于，所述石墨烯为2～50层组合片状结构，层间碳原子以π键结合，层内碳原子以sp2杂化轨道组成六角形蜂巢状晶格。
  7. 根据权利要求1所述的石墨烯改性无机涂料，其特征在于，所述石墨烯为带有官能团修饰的改性石墨烯，所述官能团为羟基、羧基、氮基、氨基中的一种或几种。
  8. 根据权利要求1所述的石墨烯改性无机涂料，其特征在于，所述石墨烯为粉末状或浆料状。
  9. 根据权利要求2所述的石墨烯改性无机涂料，其特征在于，所述纳米隔热浆料为ITO、ATO中的一种或其混合物。
  10. 一种石墨烯改性无极涂料的制备方法，其特征在于，包括步骤：
    按质量百分比计，先将50～90份的高硬度聚合物树脂和10～50份的纳米隔热浆料混合均匀，再依次加入0～10份的助溶剂、0～0.5份的消泡剂、0～0.5份的抑泡剂、0～0.5份的基材润湿剂以及0～0.5份的流平剂混合均匀； 最后加入0.001～5份的石墨烯，在500-700r/min的搅拌速度下搅拌30-80min后，得到石墨烯改性无机涂料。
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