CN102630245B - 生产含聚合物涂层的方法 - Google Patents
生产含聚合物涂层的方法 Download PDFInfo
- Publication number
- CN102630245B CN102630245B CN201080053675.2A CN201080053675A CN102630245B CN 102630245 B CN102630245 B CN 102630245B CN 201080053675 A CN201080053675 A CN 201080053675A CN 102630245 B CN102630245 B CN 102630245B
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- Prior art keywords
- carbanion
- calcium ion
- polymkeric substance
- polymeric coating
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- 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.)
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 58
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 28
- 238000011065 in-situ storage Methods 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims description 54
- 239000000126 substance Substances 0.000 claims description 39
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims description 34
- 229910001424 calcium ion Inorganic materials 0.000 claims description 34
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- 239000011521 glass Substances 0.000 claims description 5
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 5
- 238000002955 isolation Methods 0.000 claims description 5
- 239000011707 mineral Substances 0.000 claims description 5
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 229920002125 Sokalan® Polymers 0.000 claims description 4
- 229920001577 copolymer Polymers 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 3
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- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 2
- 150000001298 alcohols Chemical class 0.000 claims description 2
- 150000003973 alkyl amines Chemical class 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 2
- 229920000728 polyester Polymers 0.000 claims description 2
- 230000008569 process Effects 0.000 claims description 2
- 125000001453 quaternary ammonium group Chemical group 0.000 claims description 2
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- 239000011575 calcium Substances 0.000 description 4
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- 238000003384 imaging method Methods 0.000 description 3
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- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
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- 239000001506 calcium phosphate Substances 0.000 description 2
- 229910000389 calcium phosphate Inorganic materials 0.000 description 2
- 235000011010 calcium phosphates Nutrition 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
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- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 2
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- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
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- 238000012360 testing method Methods 0.000 description 2
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- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
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- 241000370738 Chlorion Species 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- 108090000247 Haliotis laevigata perlucin Proteins 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 206010039361 Sacroiliitis Diseases 0.000 description 1
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical class [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- 239000004902 Softening Agent Substances 0.000 description 1
- JNVCSEDACVAATK-UHFFFAOYSA-L [Ca+2].[S-]SSS[S-] Chemical compound [Ca+2].[S-]SSS[S-] JNVCSEDACVAATK-UHFFFAOYSA-L 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
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- -1 and from mycocide Substances 0.000 description 1
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- 230000003143 atherosclerotic effect Effects 0.000 description 1
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- 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
- 230000003592 biomimetic effect Effects 0.000 description 1
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- 238000009835 boiling Methods 0.000 description 1
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- FJDQFPXHSGXQBY-UHFFFAOYSA-L caesium carbonate Chemical compound [Cs+].[Cs+].[O-]C([O-])=O FJDQFPXHSGXQBY-UHFFFAOYSA-L 0.000 description 1
- 229910000024 caesium carbonate Inorganic materials 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229910001622 calcium bromide Inorganic materials 0.000 description 1
- 229940059251 calcium bromide Drugs 0.000 description 1
- WGEFECGEFUFIQW-UHFFFAOYSA-L calcium dibromide Chemical compound [Ca+2].[Br-].[Br-] WGEFECGEFUFIQW-UHFFFAOYSA-L 0.000 description 1
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- 159000000007 calcium salts Chemical class 0.000 description 1
- 229940095672 calcium sulfate Drugs 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
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- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
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- 229910052901 montmorillonite Inorganic materials 0.000 description 1
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- 239000002086 nanomaterial Substances 0.000 description 1
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- 229910052757 nitrogen Inorganic materials 0.000 description 1
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- 231100000614 poison Toxicity 0.000 description 1
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- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 1
- 235000015320 potassium carbonate Nutrition 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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- WPFGFHJALYCVMO-UHFFFAOYSA-L rubidium carbonate Chemical compound [Rb+].[Rb+].[O-]C([O-])=O WPFGFHJALYCVMO-UHFFFAOYSA-L 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/02—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
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- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
- C01F11/181—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by control of the carbonation conditions
-
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- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
- C01F11/182—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds
- C01F11/183—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds the additive being an organic compound
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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
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- C—CHEMISTRY; METALLURGY
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- C09D5/1618—Non-macromolecular compounds inorganic
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- C—CHEMISTRY; METALLURGY
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- C—CHEMISTRY; METALLURGY
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- B05D1/00—Processes for applying liquids or other fluent materials
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
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Abstract
本发明涉及一种通过将碳酸钙原位沉淀而生产用于表面的含聚合物涂层的方法。本发明还额外涉及含聚合物涂层本身以及已经施加了这类含聚合物涂层的表面。该含聚合物涂层优选具有抗菌作用。
Description
本发明涉及一种通过将碳酸钙原位沉淀而生产用于表面的含聚合物涂层的方法。本发明还额外涉及含聚合物涂层本身以及已经施加了这类含聚合物涂层的表面。含聚合物涂层优选具有抗菌作用。
涂层通常应理解为是指适合表面形状的物质的(通常)牢固的粘着层。涂层在许多用途方面,如医学、材料领域或船运方面都是重要的。
最近的涂层种类之一是纳米涂层,它指将纳米范围的颗粒例如作为喷雾或雾化涂层施加至表面上。雾化通常应理解为是指将液体分离为超细液滴,作为气溶胶(雾)分布在气体(通常是空气)中。气溶胶可包含均具有相同直径的液滴-单分散喷雾-或包括具有不同尺寸的液滴(在该情况下称作多分散喷雾)。由喷雾器产生的液滴平均尺寸对于纳米涂层的生产是关键的。原则上可涂覆所有种类的表面,如金属、玻璃、纺织品、塑料和矿物质。纳米涂层例如可用于卫生领域、植入物,作为防指纹涂层用于视觉显示单元,作为自清洁建筑表面或作为油漆保护用于汽车。
由于涂层通常还必须满足保护表面免受细菌、真菌或藻类侵袭的任务,因此防止了表面的破坏,对具有杀真菌、抗菌、除藻或抗微生物作用的涂层的需求日益增加。
Podsiadlo等人(Langmuir 2005,21(25),11915-11921)描述了具有抗微生物性能的珍珠母状纳米结构材料的逐层叠加结构的生产。涂层包含聚合物组分,如聚二烯丙基-二甲基氯化铵、聚丙烯酸、改性的钠蒙脱石和钠蒙脱土作为助剂。涂层借助重复浸渍方法生产。涂层的抗菌效应通过加入银纳米颗粒而产生。
US 2007/0254141描述了具有纳米结构的薄质涂层。合成借助协同的蒸气扩散/溶胶-凝胶法进行,其在室温下自发进行并不使用有机、生物或生物化学模板而产生有序的半导体材料,如具有高纯度的钛酸钡。所得材料为半导体、光电导体、光电、电光或电池材料。合成策略基于生物启发的低温方法,其进行了与半导体材料密切相关的分子前体的水解催化。通过改变温度,可获得不同的纳米颗粒尺寸和结构。
US 2008/0273206描述了磷酸钙的仿生矿化。在该方法中,说明了合成的矿化配合物的形成,即磷酸钙矿物沉积是原位获得的,且描述了关于其生产以及其动力学的研究。所得结果意欲用作生产减弱关节炎和/或动脉粥样硬化的药物的载体。
EP-A 1835053描述了一种生产与环境相容,具有有机晶体结构的生物矿物质,如珍珠母的方法。在借助膜浸渍方法的生产方法中,呈结晶形状的生源碳酸钙借助特定结晶膜在有机基质中体外产生。
目前方法的缺点为它们不可用于大面积涂覆,因为涂覆方法通常不以浸渍方法进行。此外,它们需要复杂的设备或用于降低温度或提高温度的额外能量,以及相当大的时间投资。此外,根据现有技术生产的抗菌涂层通常额外包含污染环境或甚至有毒的银或其它重金属。
因此,本发明的目的为提供一种以最少时间和最小成本,以工业和大面积规模使表面永久性涂覆,且所产生的含聚合物涂层应优选抗菌的方法。
该目的通过一种生产用于表面的含聚合物涂层的方法而实现,该方法包括将至少一种聚合物和通过原位沉淀形成的结晶碳酸钙施加至表面上,其中使用至少一种钙离子源和至少一种碳酸根离子源作为结晶碳酸钙的反应物。
本发明方法优选产生抗菌的含聚合物涂层。具体而言,涂层为具有杀菌作用的抗菌的含聚合物涂层。根据本领域熟练技术人员,抗菌试剂(涂层)应理解为是指至少部分或完全杀死或消除细菌,或防止细菌生长和繁殖的试剂。根据本领域熟练技术人员,具有杀菌作用的试剂应理解为是指杀死细菌的试剂。
根据本发明,用于结晶碳酸钙的反应物为至少一种钙离子源和至少一种碳酸根离子源。优选使用一种钙离子源和一种碳酸根离子源。存在于钙离子源中的钙离子与存在于碳酸根离子源中的碳酸根离子的反应形成碳酸钙。根据本发明,为了能使结晶碳酸钙原位沉淀,首先使钙离子源和碳酸根离子源相互空间分离。钙离子源和碳酸根离子源通过本领域熟练技术人员已知的用于将结晶碳酸钙原位沉淀的方法组合。原位沉淀优选在(待涂覆)表面上或在紧邻表面处,如距离不超过1米处直接进行。
更优选的是,原位沉淀在距离表面小于20cm处进行。为此,使钙离子源和碳酸根离子源相互空间分离,但同时经受喷雾工艺,特别是雾化工艺。因此,例如在喷雾工艺中产生的反应物液滴的碰撞和聚结可通过原位沉淀形成结晶碳酸钙。碰撞可在待涂覆表面上或在表面和雾化器之间的空间中直接发生,在该情况下原位形成(沉淀)的结晶碳酸钙沉积在表面上。特别优选结晶碳酸钙直接在表面上原位沉淀。
然而,在本发明方法中,原位沉淀不应理解为是指包括浸渍方法或膜方法的沉淀方法。
所用钙离子源可为钙盐,如氯化钙、氟化钙、溴化钙、碘化钙、硫酸钙、硫化钙、氢氧化钙,特别优选氯化钙。还可任选使用本领域熟练技术人员已知的其它钙离子源。
所用碳酸根离子源可为碱金属碳酸盐,如碳酸锂、碳酸钠、碳酸氢钠、碳酸钾、碳酸铷和碳酸铯,其中特别优选使用碳酸钠。当然还可使用本领域熟练技术人员已知的其它碳酸根离子源。
在特定钙离子源中钙离子的浓度可为0.01-4.0mol/L。在特定钙离子源中钙离子的浓度优选为0.1-1.0mol/L。
在特定碳酸根离子源中碳酸根离子的浓度可为0.01-4.0mol/L。在特定碳酸根离子源中碳酸根离子的浓度优选为0.1-1.0mol/L。
钙离子源和/或碳酸根离子源优选各自独立地包含至少一种溶剂。该溶剂优选为水或醇,更优选水。
根据本发明,将至少一种聚合物施加至待涂覆表面上,其中优选使用一种聚合物。聚合物通过本领域熟练技术人员已知的方法,如通过喷雾方法,特别是雾化方法而施加。可空间分离地和/或在不同时间或与通过原位沉淀形成的碳酸钙一起将聚合物施加至表面上。优选将聚合物和原位沉淀的碳酸钙一起施加。聚合物例如可在施加之前与钙离子源和/或碳酸根离子源部分或完全组合,如混合。然而,聚合物可任选与钙离子源和/或碳酸根离子源部分或完全空间分离。
所用聚合物原则上可为本领域熟练技术人员已知的所有聚合物。优选使用选自如下的聚合物:聚缩水甘油、聚缩水甘油衍生物、聚甘油、聚甘油衍生物、线性或改性的聚丙烯酸、马来酸和丙烯酸的共聚物、聚烷基胺、聚烯基胺、季铵聚合物、超支化聚酯和嵌段共聚物。
所用嵌段共聚物为控制碳酸钙形成的嵌段共聚物,如PEO-b-PMAA(聚(氧化乙烯)-嵌-聚(甲基丙烯酸))。此外,还可使用控制碳酸钙形成的蛋白质,如Lustrin、Perlucin、Ovocleidin或Ansocalcin。
通过本发明方法原位沉淀的碳酸钙的晶体尺寸优选小于10μm,特别是小于1μm。特别是当具有钙离子源和/或碳酸根离子源的溶液在表面上被喷雾方法雾化时,可获得小于1μm的晶体尺寸。因此,纳米涂层的生产也是可行的。
在本发明方法中,钙离子与碳酸根离子的比例为10:1-1:10,钙离子和碳酸根离子与聚合物的比例可为1:1-100:1。在本发明的特别优选的实施方案中,钙离子与碳酸根离子以及与聚合物的比例为10:10:1。聚合物和原位沉淀的碳酸钙之间的比例可控制表面上本发明的含聚合物涂层的性能。其优选形成包含原位沉淀且具有霰石结构的碳酸钙的含聚合物涂层。
通过使用不同聚合物,通过选择聚合物和借助原位沉淀形成的碳酸钙之间的比例,在本发明方法中可有利地直接控制所得结晶碳酸钙在优选的抗菌,含聚合物涂层中的晶体形态。因此,晶体生长可定位在空间受限的区域。此处聚合物影响或限制了晶体生长。根据如何选择含聚合物涂层的晶体形态,可使含聚合物涂层与不同表面和不同的最终用途匹配。例如,与不同使用领域的最佳调节例如可用于医学或材料领域,内部或外部领域,以及纳米涂层的控制生产。本发明的优选抗菌的含聚合物涂层可特别用于船体涂层。
在本发明涂覆方法中,在表面上提供包含至少一种聚合物和结晶碳酸钙的涂层。
根据使用领域,本发明的优选抗菌,含聚合物涂层的厚度可为0.1-100μm。
在本发明方法的特定优选实施方案中,通过将反应物和/或聚合物喷雾而将至少一种聚合物和通过原位沉淀形成的结晶碳酸钙施加至表面上,其中使用至少一种钙离子源和至少一种碳酸根离子源作为用于结晶碳酸钙的反应物。
当含聚合物涂层通过将反应物喷雾至表面上而施加时,以工业和大面积规模施用本发明方法是特别有利的,因为这可进一步减少时间投资和成本。
在用于生产优选抗菌,含聚合物的涂层的本发明方法中,可额外使用粘合促进剂。粘合促进剂的实例是本领域熟练技术人员已知的。
在一个实施方案中,本发明涂覆方法可进一步包括至少一个以下步骤:
a)将至少一种聚合物,至少一种钙离子源和/或至少一种碳酸根离子源雾化,其中至少一种聚合物任选存在于至少一种钙离子源和/或至少一种碳酸根离子源中,
b)任选将粘合促进剂施加至表面上,或
c)将含聚合物涂层干燥,
步骤a)-c)任选循环进行和/或步骤a)和b)的顺序可变换。
钙离子源和/或碳酸根离子源可优选同时或依次通过雾化由溶液施加。
优选抗菌的含聚合物涂层的生产例如可使用雾化器进行。所用雾化器例如可为一种物质的压力喷雾器、两种物质喷雾器(在该情况下雾化使用压缩气体,如空气或氮气进行)或特定超声或静电喷雾器。
雾化还可借助两种或更多种分离的雾化器,或借助能用单个雾化器使两种液体雾化的设计(如具有工作空气的三种物质喷嘴)。优选使用压力喷雾器或三种物质喷嘴。
雾化温度可为20-200℃。优选20℃至所用溶剂的沸点之间的温度。
结束该方法的用于干燥含聚合物涂层的任何操作优选在20-200℃的温度下进行。特别优选可在低温下进行的干燥方法。
本发明方法可产生具有珍珠母和/或莲花效应的含聚合物涂层。该性能可具有以下效果:可获得彩虹色闪光的,含聚合物的平涂层和/或含聚合物的防水和防污涂层。
本发明的含聚合物涂层同样应注意的是高的耐刮擦性。当涂覆方法借助喷雾方法进行时,含聚合物涂层可获得特别高的耐刮擦性。
在一个实施方案中,本发明方法产生具有重复组织结构的多层,至少两层的含聚合物涂层,其中涂层的结构和/或形态不随重量变化,但在各层中保持相同或至少表现得(非常)相似。以该方式,借助单个的循环方法,可产生非常耐久的,寿命长且稳定的含聚合物涂层。在该情况下,还提到“半永久性涂层”或“可自己再生的涂层”。该实施方案优选以喷雾方法进行。
在本发明的另一实施方案中,还可加入其它活性成分,如抗微生物物质。其实例可为银或锡化合物,以及来自杀真菌剂、除藻剂、除草剂、杀菌剂或抑制病毒生长剂的抗微生物活性物质。
在本发明方法中,还可额外使用其它添加剂或有效物质。其实例可为选自染料或颜料、荧光物质、胶质、增塑剂、稳定剂或UV稳定剂的物质。
本发明进一步提供了可通过本发明方法生产的含聚合物涂层。
本发明进一步提供了可施加可通过本发明方法生产的含聚合物涂层的表面。
本发明进一步提供了可通过本发明方法生产的含聚合物涂层,和/或已涂覆有可通过本发明方法生产的含聚合物涂层且可具有抗菌作用的表面。
根据本发明,原则上可提供具有本发明的基于碳酸钙的,优选抗菌的含聚合物涂层的所有表面,如金属、玻璃、纺织品、塑料和矿物质。
根据本发明生产的优选抗菌的含聚合物涂层例如可发现以下用途:船体涂层,水下测量仪器的涂层,潜水探测器和船舱、浮标、钻油平台的涂层,用于风轮机、发射器天线、庭院家具的涂层,用于建筑表面的漆,卫生领域制品、植入物或医学测量和储存制品的涂层。
实施例:
实施例1:
将具有用于管道线的泵压头的蠕动泵(Ismatec)用于使Schlick三种物质喷嘴填充两种不同溶液。将喷嘴安装在距离垂直滑片(玻璃)10cm处。
通常生产涂层包括三个方法步骤:
1.喷涂:用两种反应物溶液将滑片喷雾(玻璃显微镜滑片),所述反应物溶液反应并直接在滑片表面上产生CaCO3。
2.在双蒸馏水中洗涤,以除去所存在的钠和氯离子,以及未吸收的化学物质。
3.干燥(在室温下,使用空气)或热处理(在120-300℃下):空气从压缩空气供应网络中流出至滑片上;热处理在干燥箱中进行。
就涂层的生产而言,将步骤1-2或1-3重复数次。涂覆时间(步骤1)在5秒-60分钟内变化,集中在5-60秒。
为生产混合薄层,起初将钙和碳酸根离子相互分离地投入。使用以下反应物溶液:
溶液1:含聚丙烯酸的Na2CO3水溶液(Sokalan PA 30,MW=8000g/mol),
溶液2:含聚乙烯亚胺(PEI)的CaCl2水溶液(Lupasol WF;MW=25000g/mol。
Ca2+和CO3 2-的浓度在0.01-1Mol/L范围内变化,且磨耗稳定性在浓度为0.1Mol/L时获得。所选择的Ca2+:CO3 2-:COO-离子的比例为10:10:1和10:10:10。对于聚乙烯亚胺(PEI),选择20g/L的浓度。
指甲触压试验
测试表面涂层的耐磨耗性且表面涂层甚至在水和盐中也保持稳定。
实施例2:
程序与实施例1相似。
1.喷涂:喷雾时间为5秒。溶液1:0.1Mol/L Na2CO3+0.1Mol/L COO-。溶液2:0.1Mol/L CaCl2+20g/L PEI。
2.洗涤:在水中30秒。
重复步骤1和2两次。吹干300秒。重复步骤1和2。吹干300秒。
使涂层经受SEM成像和原子力显微镜分析以用于评估。它们显示了粗糙度(在三个不同样品a)-c)上测量,间断接触模式,8μm×8μm,测定均方根粗糙度Rq和波度Wq):
a)Rq=13nm±1nm Wq=83nm±13nm
b)Rq=9nm±1nm Wq=64nm±10nm
c)Rq=16nm±1nm Wq=61nm±4nm
和晶体尺寸(细节扫描1μm ×1μm):
d平均样品1=190nm±10nm
d平均样品2=150nm±12nm。
在部分边缘区域,发现非常多具有非常窄粒度分布的较细晶体(如d_p=67nm±3nm),它们已经自组织。膜厚度被测定为h=3.43±0.09μm。
实施例3:
操作与实施例1相似。
1.喷涂:喷雾时间为5秒。溶液1:0.1Mol/L Na2CO3+0.1Mol/L COO-。溶液2:0.1Mol/L CaCl2+20g/L PEI。
2.洗涤:在水中30秒。
3.在环境温度下,在空气流中干燥(300秒)。
重复步骤1-3五次。
使涂层经受SEM成像和扫描显微镜分析以用于评估。它们显示了粗糙度(在三个不同样品a)-c)上测量,间断接触模式,8μm ×8μm,测定均方根粗糙度Rq和波度Wq):
a)Rq=26nm±2nm Wq=111nm±17nm
b)Rq=17nm±3nm Wq=107nm±20nm
c)Rq=11nm±1nm Wq=75nm±13nm
和晶体尺寸(细节扫描1μm ×1μm):
d_平均样品1=185nm±11nm
d_平均样品2=152nm±9nm。
在部分边缘区域,发现非常多具有非常窄粒度分布的较细晶体(如d_p=48nm±1nm),它们已经自组织。膜厚度被测定为h=4.98±0.17μm。
实施例4:
操作与实施例1相似。
1.喷涂:喷雾时间为5秒。溶液1:0.1Mol/L Na2CO3+0.1Mol/L COO-。溶液2:0.1Mol/L CaCl2+20g/L PEI。
2.洗涤:在水中30秒。
3.在环境温度下,在空气流中干燥(300秒)。
重复步骤1-3一次。
使涂层经受SEM成像和扫描显微镜分析以用于评估。它们显示了粗糙度(在三个不同样品a)-c)上测量,间断接触模式,8μm×8μm,测定均方根粗糙度Rq和波度Wq):
a)Rq=18nm±1nm Wq=62nm±10nm
b)Rq=22nm±1nm Wq=68nm±7nm
c)Rq=23nm±4nm Wq=108nm±17nm
和晶体尺寸(细节扫描1μm×1μm):
d_平均样品1=153nm±9nm。
在部分边缘区域,发现非常多具有非常窄粒度分布的较细晶体(如d_p=58nm±3nm)。膜厚度被测定为h=1.55±0.15μm。
实施例说明耐刮擦且平坦的涂层借助本发明喷雾方法是可行的。分析说明纳米级Ca2CO3晶体借助所述方法获得且它们已嵌入聚合物底物中。
Claims (15)
1.一种生产用于表面的含聚合物涂层的方法,其包括将至少一种聚合物和通过原位沉淀形成的结晶碳酸钙施加至表面上,其中使用至少一种钙离子源和至少一种碳酸根离子源作为结晶碳酸钙的反应物,其中原位沉淀在表面上或在距离不超过1米处直接进行。
2.根据权利要求1的方法,其中所述钙离子源或碳酸根离子源包含至少一种溶剂。
3.根据权利要求2的方法,其中所述溶剂为水或醇。
4.根据权利要求1或2的方法,其中所述原位沉淀的结晶碳酸钙的晶体尺寸小于10μm。
5.根据权利要求4的方法,其中所述晶体尺寸小于1μm。
6.根据权利要求1或2的方法,其中所述含聚合物涂层具有抗菌作用。
7.根据权利要求1或2的方法,其中所述聚合物为至少一种选自以下的聚合物:聚缩水甘油、聚缩水甘油衍生物、聚甘油、聚甘油衍生物、线性或改性的聚丙烯酸、马来酸和丙烯酸的共聚物、聚烷基胺、聚烯基胺、季铵聚合物、超支化聚酯和嵌段共聚物。
8.根据权利要求1或2的方法,其中在钙离子源中钙离子的浓度为0.01-4.0mol/L或在碳酸根离子源中碳酸根离子的浓度为0.01-4.0mol/L。
9.根据权利要求1或2的方法,其中结晶碳酸钙的原位沉淀直接在表面上进行。
10.根据权利要求1或2的方法,其中在表面的含聚合物涂层中钙离子与碳酸根离子的比例为10:1-1:10,且钙离子和碳酸根离子与聚合物的比例为1:1-100:1。
11.根据权利要求1或2的方法,其中使钙离子源和碳酸根离子源相互空间分离,但同时经受喷雾工艺,且原位沉淀在距离表面小于20cm处进行。
12.根据权利要求1或2的方法,其中涂覆操作额外包括至少一个以下步骤:
a)将至少一种聚合物,至少一种钙离子源或至少一种碳酸根离子源雾化,其中至少一种聚合物任选存在于至少一种钙离子源或至少一种碳酸根离子源中,
b)任选将粘合促进剂施加至表面上,或
c)将含聚合物涂层干燥,
步骤a)-c)任选循环进行或步骤a)和b)的顺序可变换。
13.根据权利要求1或2的方法,其用于生产用于选自金属、玻璃、纺织品、聚合物和矿物质的表面的含聚合物涂层。
14.根据权利要求1或2的方法,其中所述含聚合物涂层具有珍珠母或莲花效应。
15.根据权利要求1或2的方法,其中任选将抗微生物物质加入含聚合物涂层中。
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PCT/EP2010/068273 WO2011064323A1 (de) | 2009-11-27 | 2010-11-26 | Verfahren zur herstellung von polymerhaltigen beschichtungen |
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WO2011000854A1 (de) | 2009-06-30 | 2011-01-06 | Basf Se | Verfahren zur phosphin-initialisierten herstellung von hyperverzweigten polyolen |
US9184057B2 (en) | 2011-03-18 | 2015-11-10 | Basf Se | Method for manufacturing integrated circuit devices, optical devices, micromachines and mechanical precision devices having patterned material layers with line-space dimensions of 50 nm and less |
CN102391742B (zh) * | 2011-08-09 | 2015-11-18 | 刘福州 | 一种墙体壁纸的制备方法 |
KR101938648B1 (ko) | 2012-10-23 | 2019-01-15 | 삼성전자주식회사 | 이미지 센서를 포함하는 모바일 기기, 이미지 센서의 구동 방법 및 모바일 기기의 구동 방법 |
US10308816B2 (en) * | 2014-05-05 | 2019-06-04 | Potters Industries, Llc | Coatings for pelletized thermoplastic pavement marking compositions |
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JP3913821B2 (ja) * | 1996-10-25 | 2007-05-09 | 丸尾カルシウム株式会社 | 粒子径が制御された立方体炭酸カルシウムの製造方法 |
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- 2010-11-26 WO PCT/EP2010/068273 patent/WO2011064323A1/de active Application Filing
- 2010-11-26 US US13/512,173 patent/US9011979B2/en not_active Expired - Fee Related
- 2010-11-26 KR KR1020127013586A patent/KR20120117760A/ko not_active Application Discontinuation
- 2010-11-26 JP JP2012540440A patent/JP5748763B2/ja not_active Expired - Fee Related
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US2583548A (en) * | 1948-03-17 | 1952-01-29 | Vanderbilt Co R T | Production of pigmented cellulosic pulp |
EP1916282A1 (en) * | 2005-08-03 | 2008-04-30 | Nippon Paint Marine Coatings Co., Ltd. | Water-base coating composition and coated steel sheet |
CN101541901A (zh) * | 2006-10-02 | 2009-09-23 | 奥多摩工业株式会社 | 涂布液及涂覆该涂布液的涂料纸 |
US20090192252A1 (en) * | 2008-01-30 | 2009-07-30 | John Stration | Photocatalytic coating compositions |
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CN102630245A (zh) | 2012-08-08 |
EP2504399A1 (de) | 2012-10-03 |
KR20120117760A (ko) | 2012-10-24 |
JP2013512298A (ja) | 2013-04-11 |
US20120263973A1 (en) | 2012-10-18 |
US9011979B2 (en) | 2015-04-21 |
WO2011064323A1 (de) | 2011-06-03 |
JP5748763B2 (ja) | 2015-07-15 |
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