CN1817990A - 一种高疏水性、高导热性和高粘附性界面涂料 - Google Patents
一种高疏水性、高导热性和高粘附性界面涂料 Download PDFInfo
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Abstract
一种高疏水性、高导热性和高粘附性界面涂料，其技术方案为：采用三氯乙烷，丁酮作分散介质，以减轻对人体健康和环境污染的危害；用经硅油液相处理的普通色素炭黑使之完全疏水化，以解决涂料的沉淀问题；用聚酯改性二甲基硅氧烷，使涂膜形成密排甲基表面；用超声波均质器作搅拌分散设备，以节约能源。这种界面涂料，供家用空调器中室内、外管片(1)式换热器表面处理用，所形成涂膜(2)中为固化的聚甲基苯基硅树脂的三维交联网络，其内包裹纳米级的炭黑和二氧化硅，在涂膜表面形成密排甲基薄层(3)。于是涂膜具备高粘附和高导热性，涂膜表面具有高疏水性和较好的硬度。涂膜及其表面薄层是无毒的。
Description
技术领域
本发明涉及一种金属表面用功能涂料，特别是一种压缩式空调器的蒸发器表面用的具有高疏水性、高导热性和高粘附性的功能涂料的组成。
背景技术
已有技术中，中国发明专利ZL 001 10559.0公开了一种高疏水性、高导热性和高粘附性界面涂料(以下简称：三性界面涂料)。这种三性界面涂料存在三个问题，问题一，三性界面涂料中所用的分散介质为工业甲苯，按对人体健康的损害分类，甲苯属第二类，即在一定程度上有害或稍有毒害的溶剂；按在工厂使用条件下的危害性分类，甲苯属第二类，即中毒性溶剂。根据我国1980年颁布的TJ36-79(工业企业卫生标准)，空气中甲苯蒸汽最大容许浓度(maximum allowable-concentration，MAC)为100mg/m3。三性界面涂料采用工业甲苯为分散介质，其原因是甲苯为成膜基料的良溶剂，以及价格便宜。问题二，三性界面涂料中的固体微粒分为两类：一类是强化导热性*00胶体石墨粉剂，其初始平均粒径为1.5微米(μm)，或通用型铝粉，铝粉微粒为微小鳞片状结构，厚度为0.1～2.0μm，直径为1～200μm；另一类是形态学效应的R202，它是经硅油处理的气相二氧化硅，初始平均粒径为12纳米(nm)，是完全疏水性的。这两类固体微粒的初始平均粒径相差悬殊，以*00胶体石墨粉剂与R202为例，前者与后者初始平均粒径之比为1500/12＝125。因此这种三性界面涂料的稳定性差，产生固体微粒的沉淀。问题三，原三性界面涂膜虽有成膜基料与其中固体微粒配伍好，柔韧性以及粘附力相对较强等优点，但其膜面硬度较差，疏水性不是很高。
发明内容
一种高疏水性、高导热性和高粘附性界面涂料是原三性界面涂料的继承与发展。因此，本发明的目的是对人体健康和环境的污染的危害降低至尽可能低的限度；采用固体微粒的最佳搭配，使形态学效应和强化导热性有机结合；解决涂料的稳定性；改善涂膜表面的疏水性及硬度，提出一种稳定性好、对环境污染小、硬度较高、疏水性能较好的一种高疏水性、高导热性和高粘附性界面涂料(以下简称：三性界面涂料改进型)。
本发明是用如下方法实现的。
三性界面涂料改进型的组成成份包括有成膜基料、分散介质、固体微粒和助剂。
1.成膜基料的选用，原三性界面涂料中的成膜基料是聚甲基苯基硅氧烷，聚甲基苯基硅氧烷与固体微粒的配伍性好、附着力和疏水性较好，本三性界面涂料改进型的成膜基料仍选用W33-15(聚甲基苯基硅氧烷的甲苯溶液，溶液中，聚甲基苯基硅氧烷与甲苯的质量比是1∶1，聚甲基苯基硅氧烷的R/Si＝1.47，RC6H5/RCH3＝0.48)。
2.分散介质的选用，选用对环境污染低且能与成膜基料(聚甲基苯基硅氧烷)相溶的溶剂或它们的混合溶剂。
在涂料工业中，溶剂是泛指那些用来溶解成膜基料、形成便于施工且在形成涂膜的过程中挥发掉的液体。
溶解力，作为溶剂的主要特性之一，比较科学的方法是用“溶解度参数相近的原则”进行量化。根据赫尔德布兰德(hildbrand)的定义：
δ＝(ΔE/V)1/2
式中：δ为溶解度参数，单位(J/m3)1/2，ΔE为每摩尔物质的内聚能，V为摩尔体积。从物理意义看，δ是单位体积内分子间作用力：当两种液体的δ相同，这两种液体可以互溶；当液体与固体颗粒的δ相同，则固体颗粒可以液解于溶液中，从热力学观点，液体与液体以及液体与固体颗粒混合，在定温定容条件，自发进行的方向是系统自由能的降低，按照这一原理，可以推导出，当两种物质(液体与液体，液体与固体颗粒)溶解度参数之差的绝对值|Δδ|＜2.660×103～3.683×103(J/m3)1/2时，可认为能互溶，当然|Δδ|越小互溶性就越好。由于聚甲基苯基硅氧烷的溶解度参数没能查到确切数据，这里近似取其良溶剂甲苯的溶解度参数Δδ甲苯＝18.21×103(J/m3)1/2为其参考值。
1，1，1-三氯乙烷(以下简称三氯乙烷)，示性式为CCl3CH3，它在脂肪族卤代烃中是毒性最低的物质之一。在工作场所最大允许浓度(MAC)，在美国规定为1900mg/m3，在日本规定为1100mg/m3，比甲苯100mg/m3，高出十倍以上。它的溶解度参数δCl＝19.64×103(J/m3)1/2，δCl-δ甲苯＝19.64×103-18.21×103＝1.43×103＜2.66×103，可见，三氯乙烷能溶解成膜基料。
2-丁酮(又称甲基乙基酮、甲乙酮，以下简称丁酮)，分子式为CH3COC2H5，它属于低毒类物质，在工作场所，最大允许浓度为590mg/m3，比甲苯100mg/m3，高出近五倍。丁酮不太污染环境，因为它挥发性好，在空气中容易分解为另外的物质。它的溶解度参数为δb＝19.03×103(J/m3)1/2，δb-δ甲苯＝0.82×103＜2.66×103，可见丁酮能溶解成膜基料。
粘度，分为动力粘度μ和运动粘度υ＝μ/ρ，式中ρ为密度，动力粘度和运动粘度的单位分别为Pa·s和m2/s。粘度也是溶剂的主要特性之一。按动力粘度数值大小排列，三氯乙烷、甲苯、丁酮分别为0.903mPa·s、0.5866mPa·s、0.423mPa·s。以体积比，丁酮二份，三氯乙烷一份组成的混合溶剂的动力粘度μmix＝2×0.423/3+0.903/3＝0.583mPa·s，与甲苯相接近。
挥发率，以醋酸正丁酯挥发速率为基准即取为1，按挥发速率快慢排列，丁酮、甲苯、三氯乙烷分别为4.65、1.95、1.5。
表面张力，甲苯、三氯乙烷、丁酮、分别为28.53mN/m、25.56mN/m、24.60mN/m，三者相差不大。
综上所述，由于丁酮挥发较快，不宜单独作三性界面涂料改进型的分散介质。因此，两种溶剂可选用，其一：三氯乙烷；其二：三氯乙烷和丁酮的混合溶剂。
3.固体微粒的选用，原三性界面涂料中为了强化涂膜的导热性选用平均粒径为微米(μm)级的、导热系数很高的通用铝粉或*00胶体石墨粉剂，因而造成了三性界面涂料固体微粒的沉淀现象，涂液的稳定性不好。为解决这一问题，选用纳米级的普通色素炭黑代替它们，纳米级的普通色素炭黑初始粒径为26～37nm，比表面积为80～200m2/g，保留了原三性界面涂料中经硅油处理的气相二氧化硅R202。普通色素炭黑初始平均粒径为26～37nm，它与硅油处理气相二氧化硅的粒径比26/12～37/12＝2.17～3.08，比125小多了。在由固体微粒与液体组成的系统中，如微粒与液体之间没有化学亲和力，即两者的溶解度参数Δδ＞3.680×103(J/m3)1/2，则这种系统在热力学上是不稳定的，固体微粒就会沉淀；但是从胶体化学得知，当微粒的粒径小于100nm时，这种微粒受到周围液体分子的撞击时，由于受力面积非常小而产生不平衡力，这些微粒就产生布朗(R.Brown)运动，它是一种不规则的热运动，就会使这些微粒均匀分布在液体中，因而具有动力学的稳定性。通常认为粒径小于100nm的粒子称为纳米粒子。于是气相二氧化硅和普通色素炭黑属于纳米级。但是，作为黑色颜料，在涂料工业，炭黑的分散是最为困难。这是因为炭黑是一种高分散、多孔的疏水性物质，但其表面上有多种活性官能团(羧基、羟基、羰基)，因而形成了炭黑也具有亲水性。这样，炭黑在涂料中有形成不稳定的悬浮颗粒的自发倾向，在涂料的贮存过程中，重新聚合为絮聚体(以面相接的初始粒子团)和附聚体(以点、角相接的初始粒子团)，出现返粗变稠和沉淀现象。为解决炭黑在涂料中产生的上述问题，采用硅油对炭黑进行疏水化处理，使炭黑表面上活性官能团吸附硅油，且为防止硅油和溶剂对活性官能团的竞争吸附，所用硅油不加使之稀释的任何溶剂。我国常用颜料分散设备，如三辊磨、砂磨机、高速分散机和胶体磨等，都不能使固体微粒的粒径分散至纳米级。以分散最细的胶体磨而言，其最小的分散粒径1000nm以上。超声波均质器(超声波同化器Supersonichomogenizen)，其振子在外力(交流电)作用下产生超声振动。这种振动会在周围介质中向外传播。在液态物质中传播，在一个振动周期中有半个周期压缩半个周期膨胀。由于振动很快，如2.5万赫兹(Hz)，在膨胀半周期，液体来不及膨胀而出现气泡。在压缩半周期气泡被压缩，于是气泡急崩溃，而产生空穴现象。在空穴消失的瞬间，此时的压力可达数百兆帕(MPa)，从而起着非常复杂而强烈机械搅拌作用，使液体中固体微粒逐渐分散到胶体颗粒的范围(1～100nm)。对普通色素炭黑有絮聚和附聚而形成大颗粒的炭黑通过超声波均质器的分散作用，将颗粒粒径恢复接近初始粒径26～37nm是可以做到的。这样炭黑上活性基团吸附硅油，形成完全疏水性的纳米粒子。
综上所述，固体微粒采用R202(经硅油处理的气相二氧化硅)和经硅油处理的炭黑。
4.助剂，原三性界面涂料中采用乙烯基三特丁基过氧硅烷作偶联剂，解决三性界面涂膜的高粘附性。本三性界面涂料改进型保留了原三性界面涂料中YGO-1401(浓度是40％的乙烯基三特丁基过氧硅烷甲苯溶液)作偶联剂，原三性界面涂料的成膜基料W33-15中的聚甲基苯基硅氧烷虽有与固体微粒的配伍性好和附着力相对较好的优点，但疏水性比纯甲基硅树脂差，且涂膜表面硬度差。为了克服这些缺点，在三性界面涂料改进型加入助剂增滑剂-聚酯改性二甲基硅氧烷BYK--310，它是德国BYK公司的成熟产品，在通常烘烤温度下很稳定，只在超过200℃时聚酯链才出现降解，它的添加量视用途而定，用量较少。在膜面上形成厚度仅为几个低分子的密排甲基薄层，其真实接触角为103°。
综上所述，助剂采用YGO-1401(浓度是40％的乙烯基三特丁基过氧硅烷甲苯溶液)和BYK-310(聚酯改性二甲基硅氧烷)。上述经硅油处理的炭黑用的硅油可以是硅油201-1000，为二甲基硅油，粘度为1000mm2/s(医用卫生级，上海树脂厂生产)。
根据上述对于涂料组成成份的选择，本发明的三性界面涂料改进型的组成成份包括有成膜基料、分散介质、固体微粒和助剂。
成膜基料是W33-15(聚甲基苯基硅氧烷的甲苯溶液，溶液中，聚甲基苯基硅氧烷与甲苯的质量比是1∶1，聚甲基苯基硅氧烷的R/Si＝1.47，RC6H5/RCH3＝0.48)，分散介质是三氯乙烷或三氯乙烷与丁酮的混合溶剂，固体微粒是R202(经硅油处理的气相二氧化硅)和经硅油处理的炭黑，助剂是YGO-1401(浓度是40％的乙烯基三特丁基过氧硅烷甲苯溶液)和BYK-310(聚酯改性二甲基硅氧烷)，三性界面涂料改进型的各组成成份的体积份是：W33-15：100，三氯乙烷：100～300，丁酮：0～200，R202：200～350，炭黑：200～400，YGO-1401：8～12，BYK-310：4～6，硅油201-1000：1～2。
由于综合采用了毒性很低的有机溶剂作分散介质，涂料中的固体微粒是纳米级，超声波技术以及膜面为密排的甲基，三性界面涂料改进型比原三性界面涂料有显著的进步，表现在：
1.由于采用超声波技术对涂料中的固体微粒进行分散，超声波产生空穴，周围流体对空穴强大的冲击力[数百兆帕(MPa)]很容易使固体微粒分散至初始平均粒径，气相二氧化硅的平均粒径近于12nm，普通色素炭黑平均粒径近于26～37nm。更重要的是超声波分散是在密闭的容器中进行，因此三性界面涂料改进型的生产厂家，可以实现有机溶剂的零排放；对于三性界面涂料改进型的使用厂家，如没有机溶剂的回收循环使用的设备，由于选用的有机溶剂是低毒性，对工作场所的工作人员健康和对大气的污染也大为降低。
2.由于对炭黑用硅油进行疏水性处理和随后的超声波分散，解决了原三性界面涂料中的沉淀问题。
3.由于采用微量的聚脂改性二甲基硅氧烷，在三性界面涂料改进型形成涂膜膜面疏水性有了改善且膜面硬度更强了。
4.关于超声波技术应用于涂料工业，其优点可归纳如下：
(1)超声波均质器能产生胶体磨和高速均质机的联合效果。涂料不升温、不挥发、不吸入空气。
(2)能耗低，单位能耗仅1.5KW·h/t。
(3)结构小，投资很少，几个月能回收，维修、清洗极简便。[参见S.E.Booth.Ultrasonicass as a Method of Mixing，Dispersion and Homogenisation.Paint&Resin，1986，56(6)：17～18。译文：S.E.布恩。搅拌，分散和均质的超声波法。涂料与树脂，1986，56(6)：17～18]
附图说明
附图是三性界面涂料改进型涂敷于换热器板片而形成的三性界面涂膜改进型示意图。图中1为换热器板片，2为改进型三性界面涂膜，它由固化的聚甲基苯基硅树脂三维交联网络，且其中包裹胶体粒子所组成，3是涂膜表面，它由密排的甲基组成。
具体实施方式
关于涂膜疏水性、导热性和粘附性的测定，由本发明是原三性界面涂料的改进型，首先考虑粘附性，原三性界面涂料中应用了乙烯基三特丁基过氧硅烷作为硅偶联剂，从而取得原三性界面涂膜的高粘附性，在三性界面涂料改进型仍然采用这种硅偶联剂，而且成膜基料与它的体积比(1∶0.1)不变，因而可以推论三性界面涂料改进型的涂膜仍然保持了高粘附性；关于疏水性，将涂膜水平向上放置，用2.5ml一次性注射器吸足纯净水，缓慢从针头挤出水珠直径在1mm左右，水珠仍沾在针头上，让水珠沿涂膜面缓慢移动，如水珠不沾膜面，稍稍提起针头，使水珠增大至2mm，水珠落在膜面上不能停留，即涂膜稍有倾斜或振动，水珠立即从膜面脱落，则可以为涂膜保持高疏水性，此法可称为注射器挤水珠法；关于导热性，应用电热类比，应用数字万用表(DT9203型)，其电阻为200、2k、20k、200k、2M和20M六档，将该万用两条测量导线前的尖形探头改为两片紫铜板，板宽12mm、长14mm，将这两片紫铜用胶粘在一平整电木板上，两紫铜板间的间隙为0.5mm，两板的另一侧用锡焊连接测量导线。使用时，将两紫铜板紧贴于涂膜膜面，测量其电阻值，电阻越小，则涂膜导电性越好，也表征涂膜导热性越好，此法可称为测电阻法。
实施例1：
在专利ZL 001 10559.0实施例4中，将WGS-0310应用于捷达汽车空调器的蒸发器，该蒸发器单体性能试验检测数据表明有WGS-0310涂膜较之无涂膜，空气侧能力提高了3.4％。在本发明中，将聚酯改性的二甲基硅氧烷(BYK-310)加入WGS-0310中，加入的量按为WGS-0310中成膜基料(按体积比为5％)，将加有助剂BYK-310的涂液应用于郑州日产汽车空调器中的蒸发器，在同一试验台上，蒸发器单体性能试验检测数据表明有这种涂膜较之无涂膜，空气侧能力提高了9.02％＞3.4％。可能有其他的因素，但三性界面涂料改进型中的助剂加入BYK-310，效果是正面的。
实施例2：
为了从实验上验证经硅油处理气相二氧化硅(R202，初始平均粒径12nm，白色无定形粉末)所配置的涂液的分散稳定性，是本实施例的目的。
成膜基料为W33-15，其体积以VW表示；分散介质(1)三氯乙烷，其体积以VCl表示，分散介质(2)丁酮，其体积以Vb表示；固体微粒为R202，其体积以VS表示；助剂为YGO-1401，其体积以Vv表示。这一组合物各组分的体积比为：
VW∶Vv∶VCl∶Vb∶VS＝1∶0.1∶1.5∶1.5∶5.5
上述混合物配制好后，在超声波均质器中分散1小时。涂液粘度，涂-4杯13.6秒。将载玻片[25.4×76.2mm(1″×3″)，厚1mm]浸入该涂液中，停留20秒，缓慢取出，室温晾干，放入远红外线烤箱内，在150℃时烘烤，固化成膜40分钟。涂膜的疏水性用注射器挤出水珠法，测得涂膜达到高疏水性要求；用测电阻法，测得电阻为无穷大，说明涂膜导热性很差。
将该涂液放置在500ml，广口磨砂透明玻璃瓶中，遮光静置15个月，未发现沉淀。从这个实施例中，可见完全疏水化初始粒径12nm的气相二氧化硅，在疏水的涂液中，由布朗运动而形成的胶体动力学稳定性能好，且在涂膜表面形态学效应显著。
实施例3：
成膜基料W33-15，其体积以VW表示；分散介质为三氯乙烷，其体积以VCl表示；固体微粒(1)R202，其体积以VS表示，固体微粒(2)普通色素炭黑，其体积以VC表示；助剂(1)YGO-1401，其体积以Vv表示，助剂(2)BYK-310，其体积以V310表示，(3)炭黑上活性基团吸附用硅油201-1000，为二甲基硅油，粘度为1000mm2/s(医用卫生级，上海树脂厂生产)，其体积以V201表示。
这一组合物各组分的体积比为：
VW∶Vv∶V201∶V310∶VCl∶VC∶VS＝1∶0.1∶0.01∶0.05∶3∶2∶3.5
经硅油处理的炭黑是将炭黑与二甲基硅油混合，放在超声波均质器中，将炭黑微粒分散，且炭黑微粒上的活性基团吸附硅油分子，使炭黑完全疏水化。超声波均质器工作1小时。然后将W33-15，YGO-1401以及BYK-310和三氯乙烷缓慢地注入，最后将R202加入超声波均质器中。超声波均质器工作2小时。将载玻片浸入该涂液中，缓慢取出，室温晾干，放入远红外线烤箱内，在150℃时烘烤，固化成膜40分钟。用注射器挤出水珠法，测得涂膜达到高疏水性要求；用测电阻法，测得电阻为60K，比专利ZL 00 1 10559.0实施例4，WGS-0310涂膜的电阻65K要小，说明本实施例的涂膜导热性有微小改进。
实施例4：
成膜基料W33-15，其体积以VW表示；分散介质(1)三氯乙烷，其体积以VCl表示，分散介质(2)丁酮，其体积以Vb表示；固体微粒(1)R202，以体积VS表示，固体微粒(2)普通色素炭黑，其体积以VC表示；助剂(1)YGO-1401，其体积以Vv表示，助剂(2)BYK-310，其体积以V310表示，助剂(3)炭黑活性基团吸附用硅油201-1000，为二甲基硅油，粘度为1000mm2/s(医用卫生级，上海树脂厂生产)，其体积以V201表示。这一组合物各组分的体积比为：
VW∶Vv∶V201∶V310∶VCl∶Vb∶VC∶VS＝1∶0.1∶0.02∶0.05∶1∶2∶4∶2
首先，将炭黑与二甲基硅油混合，放入超声波均质器中，将炭黑微粒分散，且炭黑微粒上的活性基团吸附硅油分子，使炭黑完全疏水化。超声波均质器工作1小时。然后将W33-15、YGO-1401、BYK-310以及三氯乙烷、丁酮缓慢地注入，最后将R202加入超声波均质器。超声波均质器工作2小时。涂液粘度，涂-4杯15.6秒。将载玻片浸入该涂液中，缓慢取出，室温晾干，放入远红外箱烤箱内，在180℃时烘烤，固化成膜40分钟。用注射器挤出水珠法，测得该涂膜达到高疏水性要求；用测电阻法，测得电阻为2.8K，远小于原WGS-0310涂膜的65K，说明本实施例的涂膜导热性有显著的改进，其原因本实施例中炭黑与成膜基料的体积比为4∶1，而实施例3中炭黑与成膜基料的体积为2∶1，即涂膜中炭黑所占的份额提高了一倍。
由于此涂液显示了三性界面涂料改进型的优点，故命名为WCS-05。附图是WCS-05涂敷于板片而生成的涂膜，图中1表示板片，2表示改进型三性界面涂膜，它是固化的聚甲基苯基硅树脂三维交联网络，且其中包裹完全疏水化的二氧化硅和炭黑的胶体粒子，3表示涂膜表面，它是密排的甲基组成。涂膜及其表面是完全无毒性的。
实施例5：
将WCS-05涂敷于50×50mm的试件(用1000号砂纸打磨，再用二甲苯除油脂的PS板)上，烘干成膜，用导热硅胶粘附半导体冷台的冷端，垂直放置，启动半导体冷台，使之在结露工况运行，连续运行8个月，运行时间为8×30×24＝5760h。
按生产厂家对家用空调规定的使用寿命为10年，每年工作180天，每天工作6小时，对冷、暖空调而言，夏季室内换热器为蒸发器(送冷风)，冬季则为冷凝器(送热风)，因此10年寿命对室内、外作为蒸发器累积工作时间应乘以0.5，即10×180×6×0.5＝5400h。
当半导体冷台运行结束时，观察涂膜未见剥落、裂纹等问题，且试件上水珠的形态与刚结露时，目测未见变化。由于5760＞5400，且为连续运行，所以改进型三性界面涂膜寿命与整机寿命相匹配。而且，从实验上使具体实施方式第一段中关于涂膜高粘附性的推论得以验证。
Claims (3)
1.一种高疏水性、高导热性和高粘附性界面涂料，其组成成份包括有成膜基料、分散介质、固体微粒和助剂，成膜基料是W33-15，固体微粒有R202，助剂有YGO-1401，其特征在于：其组成成份中分散介质是三氯乙烷或三氯乙烷与丁酮的混合溶剂，固体微粒有经二甲基硅油处理的炭黑，助剂有BYK-310，各组成成份的体积份是：W33-15：100，三氯乙烷：100～300，丁酮：0～200，R202：200～350，炭黑：200～400，YGO-1401：8～12，BYK-310：4～6，二甲基硅油201-1000：1～2。
2.根据权利要求1所述的高疏水性、高导热性和高粘附性界面涂料，其特征是：所述的各组成成份的体积份是：W33-15：100，三氯乙烷：300，R202：350，炭黑：200，YGO-1401：10，BYK-310：5，硅油201-1000：1。
3.根据权利要求1所述的高疏水性、高导热性和高粘附性界面涂料，其特征是：所述的各组成成份的体积份是：W33-15：100，三氯乙烷：100，丁酮：200，R202：200，炭黑：400，YGO-1401：10，BYK-310：5，硅油201-1000：2。
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