CN1095981A - 带有能量固化的热熔底涂层的涂敷磨料制品 - Google Patents
带有能量固化的热熔底涂层的涂敷磨料制品 Download PDFInfo
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Abstract
一种由衬材、衬材上的第一粘合剂和在第一粘合
剂中的大量磨料颗粒构成的涂敷磨料制品。第一粘
合剂是一种热熔压敏型粘合剂,它受能量固化形成交
联的涂层。本发明还涉及制备这种制品的方法。
Description
本发明涉及涂敷磨料制品,更具体地说,本发明涉及带有能量固化的热熔底涂层的涂敷磨料制品。
涂敷磨料制品一般包含一个衬层,衬层上粘结着大量的磨料颗粒。在一种形式里,磨料颗粒通过通常称为底涂层的第一粘合剂粘结在衬材上。然后将通常称为定型涂层的第二粘合剂施加在底涂层和磨料颗粒之上,以加固这些颗粒。在第二种形式里,磨料颗粒分散在粘合剂中形成磨料组合物,此磨料组合物靠粘合剂粘结在衬材上。
经常使用多孔的布、织物和纺织品作为涂敷磨料制品的衬材。底涂层通常以低粘性物质的形式涂敷到衬材上。在这种条件下,底涂层可以移动到衬材内部并且累积在由多孔衬材的交叉纱线和填充纤维形成的空隙里。这会使衬材变得刚性、坚硬和发脆,结果是丧失了它的原有的柔韧性。但是,涂敷磨料制品要求具有柔韧性和易弯性。因此,通常都采用填孔涂层或饱和涂层来封闭多孔衬材,尽管这一附加的加工步骤增加了成本和制造的复杂性。
美国专利4,163,647“制造涂敷磨料的方法”(1979年8月7日授予H.J.Swiatek)提出在布料衬材的前表面涂上一种液体的热固性树脂,其涂敷方式使树脂不透入布料的间隙中。所提议的液体热固性树脂包括可加热硬化的酚醛树脂。
美国专利4,751,138“具有可辐射固化粘合剂的涂敷磨料”(1988年6月14日授予M.L.Tumey等)公开了一种可辐射固化的环氧基底涂层。据报道,这种可辐射固化的组合物可以用来处理衬材,例如将衬材浸渍饱和或形成一个前涂层。
美国专利4,927,431“涂敷磨料的粘合剂”(1990年5月22日授予S.J.Buchanan等)公开了一种磨料制品,其中使用由可辐射固化的单体与可加热固化的树脂材料的掺混物形成的粘合剂,粘合剂将磨料颗粒粘结到衬材片的主表面上,而且还可以对涂敷磨料制品起衬材处理剂的作用。
美国专利4,240,807“用来制造砂带的带有热塑性粘合剂涂层的基底和用它制成的砂带”(1980盾12月23日授予F.J.Kron Zer)公开了一种柔性的衬材,在它的一个表面上有一种热活化的粘合剂。据报道,此粘合剂在室温下是一种不发粘的固体,但是在受热时转化成粘性流体,使得沉积于其上的磨料颗粒能在涂层中下沉一定的深度,与涂层形成牢固的结合。当停止加热后,涂层转化成固态的不发粘的状态。
但是,仍然十分需要一种底涂层,它容易涂敷在多孔的布料、织物或纺织品衬材上,而不需要用一个分离的填孔涂层或饱和涂层来密封衬材。
一般来说,本发明涉及一种涂敷磨料制品,它包括一个衬材,衬材上的第一粘合剂或底涂层,以及在第一粘合剂中的大量的磨料颗粒。很多涂敷磨料制品还包含在第一粘合剂和磨料颗粒上的第二粘合剂(例如胶或固化的树脂型粘接剂),以及在第二粘合剂上的第三粘合剂。
第一粘合剂是一种热熔压敏型粘接剂,它已被能量固化以形成交联的涂层。因为第一粘合剂是一种热熔组合物,所以它特别适用于多孔的布料、纺织品或织物的衬材。第一粘合剂不会透入多孔衬材的空隙,从而保留了衬材的原有柔韧性和易弯性。
在本发明的更概括的情况,第一粘合剂包含一种含环氧基的物质、一种聚酯组分和有效数量的一种引发剂用于粘合剂的能量固化。更具体地说,第一粘合剂含有约2至95份含环氧物质和相应地约98到5份聚酯组分,以及引发剂。还可以含有一种可任意使用的羟基官能度大于1的含羟基物质。
聚酯组分的Brookfield粘度(121℃)以超过10000毫帕·秒为宜,数均分子量约为7500到200000,约为10000到50000更好,最好是从约15000到30000。聚酯组分可以是二羧酸与二元醇的反应产物,这些二羧酸选自含有4到12个碳原子的饱和的脂族二羧酸(及其二酯衍生物)和含有从8到15个碳原子的芳族二羧酸(及其二酯衍生物),二元醇则含有2到12个碳原子。
任选使用的含羟基物质的羟基官能度以至少2为宜,羟基官能度为3则更好。特别优选的物质是聚亚氧烷基多元醇,例如数均当量约为31到2250的聚氧乙烯二醇和聚氧丙烯二醇,以及数均当量约为80到350的聚氧乙烯三醇和聚氧丙烯三醇。当引发剂是芳香锍配盐或芳香碘鎓配盐时,聚亚氧烷基多元醇特别优选。也可以使用环己烷二甲醇,尤其是如果引发剂是金属茂盐时。含羟基的物质在增强第一粘合剂的柔性方面有用,而且能充分地减慢第一粘合剂暴露于能量作用之后的固化反应,从而使磨料颗粒能与其粘结。
在更优选的第一粘合剂中,含环氧物质构成了其中的2到80份,聚酯组分则相应地构成其中的98到20份。最好是第一粘合剂中含2到60份含环氧物质和相应地从98到40份的聚酯组分。
本发明还涉及一种形成这种涂敷磨料制品的方法。将能量固化的热熔压敏型第一粘合剂敷加到(最好是涂布)衬材上并暴露于能量(优选光化辐射)之下。在第一粘合剂暴露于能量下之前或之后,将大量磨粒沉积在第一粘合剂中。然后使粘合剂固化,形成交联的涂层。第一粘合剂的压敏性质(在它最后固化之前)使得磨料颗粒能与其粘结。第一粘合剂可以加热后固化。
参考以下附图将会更充分地理解本发明,在这些图中类似的参考数字代表相同或类似的组分,其中:
图1是根据本发明的涂敷磨料制品的透视图;
图2是根据本发明的涂敷磨料制品沿图1线2-2取的截面图。
现在注意附图,图1和2画出了根据本发明的涂敷磨料制品,其中包括一个衬材12和粘结于其上的磨料层14。
衬材12可以由布、硬化纸板、纸、非织造材料、聚合物薄膜和它们的多层层压组合物构成。布衬材可以是编织的或缝编的,可以包括棉、聚酯、人造丝、丝、尼龙或其掺混物的纤维或纱线。非织造的衬材可以包括纤维素纤维、合成纤维或它们的掺混物。如同下面所解释的,在本发明的涂敷磨料中使用多孔的布、织物或纺织品衬材特别有利。
磨料层14含有大量的磨料颗粒16,它们被第一粘合剂或底涂层18粘结到衬材12的主表面上。在磨料颗粒和底涂层之上敷加第二粘合剂或定型涂层20以加固颗粒。磨料颗粒的粒度通常约为0.1到1500微米(μm),从约1到1300μm则更好。磨料颗粒的莫氏(MOH)硬度以至少约8为宜,最好是大于9。适用的磨料的实例包括氧化铝基材料(例如氧化铝、陶瓷氧化铝(它可以含有一种或多种金属氧化物改性剂)和热处理过的氧化铝)、碳化硅、共熔的氧化铝-氧化锆、金刚石、二氧化铈、立方一氮化硼、石榴石和它们的掺混物。磨料颗粒还包括诸如美国专利4,652,275和4,799,939中公开的磨料团聚体,该专利在本文中引用作为参考。
适合用于本发明涂敷磨料制品中的第一粘合剂包括一种热熔压敏型粘接剂组合物,它在能量作用下固化,形成共价交联的热固型底涂层。因为底涂层可以以热熔组合物的形式敷加,所以它不容易透入衬材,从而兼顾了衬材固有的柔韧性和易弯性。因此,本发明公开的底涂层在与多孔的布、织物或纺织品衬材一起使用时特别有利。
“多孔的”是指上面没有磨料层、底涂层、粘接剂层、密封剂、饱和涂层、填孔涂层、背面胶层等的衬材,在按照联邦试验方法标准No.191,方法5452(1968年12月31日公布)(参看E.R.Kaswell的Wellington Sears Handbook of Industrial Taxtiles,1963年版,575页)用Gurley渗透计(可自Teledyne Gurley公司得到,Tropy,New York)测得的Gurley孔度小于50秒。目前已知的涂敷磨料制品的布衬材通常需要特殊处理,例如要有饱和涂层、填孔涂层、背面胶层或底胶层以保护布料纤维并密封住衬材。但是本发明的涂敷磨料制品不需要这种处理,却仍然保持耐用和柔韧。虽然本发明的涂敷磨料制品不需要这些处理,但是如果愿意,可以作这些处理。本发明的热熔底涂层可以提供这种处理。
这种热熔底涂层的压敏型粘结性能使得磨料颗粒能粘结到底涂层上,直到在上面涂敷上定形涂层。这种交联的热固性底涂层很坚固,但仍有柔性,而且自动地粘结到衬材上。
这里所用的“热熔”组合物是指一种组合物在室温下(约20到22℃)是固体,但在受热时熔化成粘性液体。它容易施加在涂敷磨料制品的衬材上。本发明的热熔底涂层最好是配制成无溶剂的体系(即,它们在固态时溶剂含量少于1%)。这里所用的“压敏型粘结剂”是指一种热熔组合物,它在磨料颗粒施加于其上时显示出压敏性质。压敏性质意味着,作为对施加的至少是轻微的压力的响应,刚涂敷在衬材上并且仍然温热的组合物(在某些情形下甚至在冷却到室温之后)是粘性的。
适合用在本发明中的热熔底涂层包含,而且最好是基本上由以下组分构成:对底涂层的韧性和耐久性起作用的含环氧物质,使底涂层显示压敏性质的聚酯组分和使组合物在受能量作用时能够固化的一种引发剂,还可以任意地而且最好是在本发明的热熔底涂层中包含一种含羟基的物质,以延缓固化速度和/或使底涂层具有柔顺性。
适合用于本发明底涂层中的含环氧物质是分子中含有至少一个可以通过开环反应聚合的环氧乙烷环(即,
)的任何有机化合物。这些物质统称为环氧化合物,包括单体的和聚合的环氧化合物,可以是脂族、脂环族或芳族化合物。它们可以是液体或固体,或是固体与液体的掺混物,掺混物适合形成粘性的粘结薄膜。这些物质一般每分子子平均有至少两个环氧基(最好是每分子有两个以上的环氧基)。聚合的环氧化合物包括有末端环氧基的直链聚合物(例如聚亚氧烷基二醇的二环氧甘油醚)、有环氧乙烷单元骨架的聚合物(例如聚丁二烯聚环氧化物)和有侧链环氧基的聚合物(例如甲基丙烯酸缩水甘油聚合物或共聚物)。含环氧物质的分子量可以从58到约10000或更高变化。各种含环氧物质的混合物也可以用在本发明的热熔组合物中。每个分子中环氧基的“平均数”定义为含环氧物质中的环氧基数除以环氧分子的总数。
适用的含环氧物质包括含氧化环己烯基团的化合物,例如环氧环己烷羧酸酯,其实例为3,4-环氧环己基甲基-3,4-环氧环己烷羧酸酯,3,4-环氧-2-甲基环己基甲基-3,4-环氧-2-甲基环己烷羧酸酯和二(3,4-环氧-6-甲基环己基甲基)己二酸酯。这类适用的环氧化合物的更详细的名单可参见美国专利3,117,099。
特别适合用来实施本发明的其它含环氧物质包括以下化学式的缩水甘油醚单体
其中R′是烷基或芳基,n是从1到6的整数。实例有通过多元酚与过量氯乙醇(例如表氯醇)反应得到的多元酚缩水甘油醚(例如2,2-二(2,3-环氧丙氧酚)丙烷的二环氧甘油醚)。可以用来实施本发明的这类环氧化合物的其它实例见美国专利3,018,262的说明。
有许多可用于本发明的市售的含环氧物质。具体地说,容易得到的环氧化合物包括氧化十八碳烯、表氯醇、氧化苯乙烯、氧化乙烯基环己烯、缩水甘油、甲基丙烯酸缩水甘油酯、双酚A的二环氧甘油醚(例如壳牌化学公司的EPON828、EPON1004和EPON1001F,和DOW化学公司的DER-332和DER-334),双酚F的二环氧甘油醚(例如Ciba-Geigy公司的ARALDITE GY281),二氧化乙烯基环己烯(例如联合碳化物公司的ERL4206),3,4-环氧环己基甲基-3,4-环氧环己烯羧酸酯(例如联合碳化物公司的ERL-4221),2-(3,4-环氧环己基-5,5-螺-3,4-环氧)环己烷-间二噁烷(例如联合碳化物公司的ERL-4234),二(3,4-环氧环己基)己二酸酯(例如联合碳化物公司的ERL-4299),二氧化二戊烯(例如联合碳化物公司的ERL-4269),环氧化聚丁二烯(例如FMC公司的OXIRON2001),含环氧官能的硅树脂,环氧硅烷(例如β-(3,4-环氧环己基)乙基三甲氧基硅烷和γ-缩水甘油氧丙基三甲氧基硅烷,可自联合碳化物公司购得),阻燃环氧树脂(例如DER-542,DOW化学公司的一种溴化双酚型环氧树脂),1,4-丁二醇二环氧甘油醚(Ciba-Geigy公司的ARALDITE RD-2),以氢化双酚A表氯醇为基础的环氧树脂(例如壳牌化学公司的E-PONEX1510)和可熔可溶性酚醛树脂(Novolak)的聚缩水甘油醚(例如DOW化学公司的DEN-431和DEN-438)。
适用的聚酯组分包括以羟基和以羧基结尾的两种物质,它们可以是无定形或半晶态。优选使用以羟基结尾的物质。“无定形”意味着物质具有玻璃化转变温度,但是用示差扫描量热法(DSC)测量不出晶体熔点。玻璃化转变温度最好是低于引发剂的分解温度(以后讨论),但是不超过约120℃。“半晶态”是指聚酯组分用DSC方法显示出晶体熔点,最好是最高熔点约150℃。
聚酯组分的粘度在形成热熔底涂层方面起重要作用(与室温下具有可测量的粘度的液态底涂层不同)。因此,适合用在本发明的底涂层中的聚酯组分的Brookfield粘度(121℃)最好是超过10000毫帕·秒。粘度与聚酯组分的分子量有关优选的聚酯组分的数均分子量约为7500至200000,约10000至50000更好,最好是从约15000到30000。
适合用在本发明底涂层中的聚酯组分包括二羧酸(或其二酯衍生物)和二元醇的反应产物。二酸(或其二酯衍生物)可以是含有4到12个碳原子的饱和脂肪酸(包括直链、支链或环中有5到6个原子的成环物质)和/或含8到15个碳原子的芳香酸。合适的脂族酸的实例有丁二酸、戊二酸、己二酸、庚二酸、辛二酸、壬二酸、癸二酸、1,12-十二烷双酸、1,4-环己烷二羧酸、1,3-环戊烷二羧酸、2-甲基丁二酸、2-甲基戊二酸、3-甲基己二酸等。合适的芳香酸包括对苯二甲酸、间苯二甲酸、邻苯二甲酸、4,4′-二苯酮二羧酸、4,4′-二苯基甲烷二羧酸、4,4′-二苯醚二羧酸-4,4′-二苯基硫醚二羧酸和4,4′-二苯胺二羧酸。这些二酸中两个羧基之间的结构以只含碳原子和氢原子为佳,最好是一个亚苯基。任何上述二酸的掺混物均可使用。
二元醇包括有2到12个碳原子的支链、直链和环状的脂族二元醇,例如1,2-乙二醇、1,3-丙二醇、1,2-丙二醇、1,4-丁二醇、1,3-丁二醇、1,5-戊二醇、2-甲基-2,4-戊二醇、1,6-己二醇、1,8-辛二醇、环丁烷-1,3-二(2′-乙醇)、环己烷-1,4-二甲醇、1,10-癸二醇、1,12-十二烷二醇和新戊二醇。也可以使用长链二醇,包括其中的亚烷基含2到9个碳原子(优选2到4个碳原子)的聚亚氧烷基二醇。任何上述二醇的掺混物均可使用。
适用的市售羟基结尾的聚酯材料包括Huls America公司的各种饮和直链的半晶态共聚酯,例如DYNAPOL S1402、DY-NAPOL S1358、DYNAPOL S1277、DYNAPOL S1229和DYNAPOL S1401。Huls America公司的合适的直链、饱和、无定形的共聚酯包括DYNAPOL S1313和DYNAPOL S1430。
引发剂起促进热熔底涂层的固化或共价交联的作用。引发剂可以被电磁辐射(例如波长在电磁光谱的紫外或可见区域内的光)、加速粒子(例如电磁辐射)或热(例如热或红外辐射)活化。引发剂最好是光活性的,即,它们是光化辐射(波长在电磁光谱紫外或可见部分内的辐射)活化的光引发剂。
适合用于本发明底涂层的引发剂通常有三类,即,芳族碘鎓配盐、芳族锍配盐和金属茂盐。最好是选择这三类作为光引发剂。
适用的芳族碘鎓配盐具有以下化学式:
其中Ar1和Ar2是有4到20个碳原子的芳族基团,选自苯基、噻吩基、呋喃基和吡唑基。Z选自氧、硫;
R是芳基(有6到20个碳原子,例如苯基)或酰基(有2到20个碳原子,例如乙酰基、苯甲酰等);一个碳-碳键;或是
,其中R1和R2选自氢、有1到4个碳原子的烷基和有2到4个碳原子的链烯基。m的值是0或1,X是一个含卤素的配阴离子,选自四氟硼酸基、六氟磷酸基、五氟羟基锑酸基、六氯砷酸基和六氯锑酸基。
Ar1和Ar2芳基可以任意地有一个或多个稠合的苯并环(例如萘基、苯并噻吩基、二苯并噻吩基、苯并呋喃基、二苯并呋喃基等)。如果需要,芳基也可以被一个或多个非碱性基团取代,条件是它们基本上没有与环氧化物和羟基官能度反应的活性。
在美国专利4,256,828中有对于适用的芳族碘翁配盐的更全面的说明。优选的芳族碘鎓配盐是二芳基碘鎓六氟磷酸盐和二芳基碘鎓六氟锑酸盐。
适合用在本发明底涂层中的芳族碘鎓配盐只在光谱的紫外范围才是光敏的。但是,对于已知的可光解的有机卤化合物,它们可以被敏化剂敏化到光谱的近紫外区和可见区。敏化剂的实例包括芳香胺和有色的芳族多环烃类。
适合用在本发明底涂层中的芳族锍配盐可以由以下化学式确定
其中R3、R4和R5可以相同或不同,条件是至少一个基团是芳族基团。这些基团可以选自有4到20个碳原子的芳基(例如取代和未取代的苯基、噻吩基和呋喃基)和有1到20个碳原子的烷基。“烷基”一词包括取代的烷基(例如卤素、羟基、烷氧基、芳基取代的烷基)。最好是R3、R4和R5均为芳基。Z、m和x全都如上面对碘鎓配盐的定义。
如果R3、R4或R5是芳基,它可以任意地有一个或多个稠合的苯并环(例如萘基、苯并噻吩基、二苯并噻吩基、苯并呋喃基、二苯并呋喃基等)。如果需要,这些芳族基团还可以被一个或多个对于环氧化物和羟基官能度基本上无活性的非碱性基团取代。
三芳基取代的盐,例如三苯基锍六氟锑酸盐,是优选的锍盐。合适的锍配盐在美国专利4,256,828中有更全面的说明。
适合用在本发明中的芳族锍配盐本来仅在光谱的紫外区具有光敏性。但是,它们可以被例如美国专利4,256,828中提到的精选的一类敏化剂敏化到近紫外和可见区。
适用的金属茂盐具有以下化学式:
其中::
MP代表选自Cr、Mo、W、Mn、Re、Fe和Co的一种金属;
L1代表1或2个提供π电子的配位体,它们可以是相同或不同的配位体,选自取代和未取代的η3-烯丙基、η5-环戊二烯基和η7环庚三烯基,以及选自η6-苯和取代的η6-苯化合物的η6-芳族化合物和有2到4个稠合环的化合物,它们都能向MP的价电子层提供3到8个π电子;
L2代表0或者1到3个提供偶数σ电子的配位体,它们可以是相同或不同的配位体,选自一氧化碳或亚硝鎓离子;
条件是由L1和L2提供给MP的总电子电荷加上在金属MP上的离子电荷造成配合物有净的残余正电荷q,而且
q是数值为1或2的整数,代表配阳离子的残余电子电荷;
Y是选自AsF-6、SbF-6和SbF5OH-的含卤配阴离子;
r是数值为1或2的整数,代表为中和配阳离子上电荷q所需的配阴离子数。
适用的金属茂盐在美国专利5,089,536中有更全面的说明。金属茂盐引发剂最好与促进剂一起(例如叔醇的乙二酸酯)使用,但并非一定要用。促进剂最好构成以含环氧物质和聚酯组分的重量和为基础的底涂层的约0.1%到4%,约占金属茂引发剂重量的60%则更好。
适用的商品引发剂包括FX-512(一种芳族锍配盐,3M公司)、UVI-6974(一种芳族锍配盐,联合碳化物公司)和IR-GACURE261(一种金属茂配盐,Ciba-Geigy公司)。
本发明的热熔底涂层还可以任意地含有一种含羟基物质。这种含羟基物质可以是有至少1个、优选至少2个、最好是约3个羟基官能度的任何液体或固体有机物质。这种含羟基有机物质应当不含其它的含“活泼氢”的基团,例如氨基和巯基。这种含羟基的有机物还应当基本上不含可能热不稳定或光解不稳定的基团,因此此物质在低于约100℃下或者在固化期间暴露于能量来源之下时不会分解或放出挥发性组分。此有机物质优选含有两个或多个脂族伯羟基或仲羟基(即,羟基直接与非芳香碳原子链合)。这些羟基可以定位在末端,也可以作为聚合物或共聚物的侧基。含羟基物质的数均当量优选约31到2250,更优选约80到1000,最优选约80到350。
合适的有1个羟基官能度的有机物质的典型实例包括链烷醇、聚亚氧烷基二醇的单烷基醚和亚烷基二醇的单烷基醚。
合适的单体多羟基有机物质的典型实例包括亚烷基二醇(例如1,2-乙二醇、1,3-丙二醇、1,4-丁二醇、2-乙基-1,6-己二醇、1,4-环己烷二甲醇、1,18-二羟基十八烷和3-氯-1,2-戊二醇)、多羟基链烷烃(例如甘油、三羟甲基乙烷、季戊四醇和山梨醇)以及其它的多羟基化合物,例如N,N-二(羟乙基)苯甲酰胺、2-丁烯-1,4-二醇、蓖麻油等。
适用的含羟基聚合物的典型实例包括聚亚氧烷基多元醇(例如聚氧乙烯和聚氧丙烯二醇和三醇,二醇的当量为31到2250,三醇为80到350)、各种分子量的聚亚氧丁基二醇、羟基结尾的聚酯和羟基结尾的聚内酯。
适用的市售含羟基物质包括POLYMEG系列(QO化学公司)的聚亚氧丁基二醇,例如POLYMEG650、1000和2000;TERATHANE系列(杜邦公司)的聚亚氧丁基二醇,例如TERATHANE650、1000和2000;POLYTHF,BASF公司的一种聚亚氧丁基二醇;BUTVAR系列(Monsanto公司)的聚乙烯醇缩乙醛树脂,例如BUTVAR B-72A、B-73、B-76、B-90和B-98;TONE系列(联合碳化物公司)的聚己酸内酯多元醇,例如TONE0200、0210、0230、0240和0260;DESMOPHEN系列(Miles公司)的饱和聚酯多元醇,例如DESMOPHEN2000、2500,2501、2001KS、2502、2505、1700、1800和2504;RUCOFLEX系列(RUCO公司)的饱和聚酯多元醇,例如S-107、S-109、S-1011和S-1014;VORANOL234-630,Dow化学公司的一种三羟甲基丙烷;VORANOL230-238,Dow化学公司的一种甘油聚氧丙烯加成物;SYNFAC系列(Milliken化学公司)的聚氧烷基化双酚A,例如SYNFAC8009、773240、8024、8027、8026和8031;以及ARCOL系列(Arco公司)的聚氧丙烯多元醇,例如ARCOL425、1025、2025、42、112、168和240。
本发明的底涂层中含羟基有机物质的用量可以在很广范围内变化,这取决于多种因素,例如含羟基物质与含环氧物质和聚酯组分的相容性,含羟基物质的当量和官能度,以及对最终的固化底涂层所要求的物理性能。
这种可任意加入的含羟基物质在调节本发明热熔底涂层的柔性方面特别有用。随着含羟基物质的当量的增加,热熔底涂层的柔性也相应增加,但是在粘结强度方面可能会有些损失。类似地,当量减小会造成柔性的减小,而粘结强度则因而增加。因此,要选择含羟基物质的当量以使这两种性质平衡。
如果用含羟基物质调节热熔底涂层的柔性,特别优选二醇当量约为31到2250、三醇当量约为80到350的聚氧乙烯二醇和三醇。更为优选的是羟基官能度大于2、二醇当量约为31到2250、三醇当量约为80到350的聚氧丙烯二醇和三醇。当引发剂是芳族碘鎓配盐或芳族锍配盐时,使用聚亚氧烷基多元醇最为有利。如果使用金属茂盐作为引发剂,1,4-环己烷二甲醇是特别优选的柔软剂。
正如后面要详细解释的,将聚醚多元醇掺加到本发明的热熔底涂层中对于调节底涂层暴露在能量作用下的固化速度特别理想。适合用来调节固化速度的聚醚多元醇(即,聚亚氧烷基多元醇)包括聚氧乙烯和聚氧丙烯二醇和三醇,其二醇的当量约为31到2250,三醇约为80到350,以及各种分子量的聚亚氧丁基二醇和聚氧烷基化的双酚A。作为固化抑制剂的聚醚多元醇最好与芳族碘翁配盐和芳族锍配盐一起使用。金属茂盐引发剂本身就产生延缓的固化效应,不需要通过加入聚醚多元醇来进一步减速。
本发明的热熔底涂层每100份总量中含有2到95份含环氧物质,以及相应地含98到5份聚酯组分。更优选的是,本发明的热熔底涂层含有2到80份含环氧物质,以及相应地含98到20份聚酯组分。提高含环氧物质对聚酯组分的相对含量会形成更刚性的底涂层。因此,这两种组分的相对数量要根据所要求的最终底涂层的性质进行平衡。
引发剂的用量的含环氧物质和聚酯组分重量和的约0.1%至4%。增加引发剂的用量使固化加速,但是要求热熔涂层涂成较薄的一层,以避免只在表面处固化。增加引发剂的用量还使所需的作用能量减小和在施用温度下的容许放置时间缩短。引发剂的数量由底涂层应有的固化速度、能源的强度和底涂层的厚度决定。
可任意使用的含羟基有机物质的相对数量参考热熔底涂层中的羟基数目与环氧基数目之比决定。此比例的范围可以从0∶1到1∶1,优选从约0.4∶1到0.8∶1。大量的含羟基物质会提高热熔底涂层的柔性,但会造成粘结强度下降。如果含羟基物质是聚醚多元醇,其数量的增加会进一步减慢固化过程。
定型涂层20施加在磨料颗粒16和底涂层18之上。定型涂层可以含有一种胶或一种固化的树脂型粘结剂。合适的树脂型粘结剂包括酚醛树脂、氨基塑料树脂、聚氨酯树脂、丙烯酸化聚氨酯树脂、环氧树脂、丙烯酸化环氧树脂、异氰脲酸酯树脂、丙烯酸化的异氰脲酸酯树脂、烯属不饱和树脂、脲醛树脂、双马来酰亚胺和芴改性的环氧树脂,以及它们的混合物。定型涂料的前体还可以含有催化剂和/或固化剂,以便引发和/或加速下面提到的固化过程。定型涂层要根据所要求的最终涂敷磨料制品的特性来选择。
底涂层和定型涂层都可以另外含有各种可任意加入的添加剂,例如填料、研磨助剂、纤维、润滑剂、润湿剂、表面活性剂、颜料、消泡剂、染料、偶合剂、增塑剂和悬浮剂,只要它们对底涂层(在它完全固化之前)的压敏粘结性质没有不利影响,也不会破坏底涂层在暴露于能量之下时的固化能力。适用的填料的实例包括碳酸钙、偏硅酸钙、二氧化硅、硅酸盐、硫酸盐和它们的混合物。适合用在本发明中的研磨助剂包括水晶石、铵水晶石和四氟硼酸钾。
磨料层14还可以含有第三种粘合剂或超定型涂层22。一种适用的超定型涂层含有研磨助剂(例如四氟硼酸钾)和粘结剂(例如环氧树脂)。可以包含超定型涂层22以防止或减少碎屑(从加工件上磨下的物质)在磨粒之间累积,这种碎屑的累积会大大降低磨料制品的切削能力。适合用于防止碎屑累积的物质包括脂肪酸的金属盐(例如硬脂酸锌)、脲醛树脂、蜡、矿物油、交联的硅烷、交联的硅氧烷、含氟化学物和它们的混合物。
在衬材12上可以形成一个任意的背面胶层24,例如含有一种树脂型粘合剂和分散于其中的填料颗粒的防滑层,或是用来将涂敷磨料制品粘在支承板上的压敏型粘合剂。合适的压敏型粘结剂的实例包括胶乳、丝网、松香,丙烯酸酯聚合物(例如聚丙烯酸丁酯和聚丙烯酸酯)、丙烯酸酯共聚物(例如丙烯酸异辛酯/丙烯酸)、乙烯基醚(例如聚乙烯基正丁醚)、醇酸树脂粘结剂、橡胶粘结剂(例如,天然橡胶、合成橡胶和氯化橡胶),以及它们的混合物。
背面胶层还可以是一种导电物质,例如五氧化二钒(例如在磺化的聚酯中),或是碳黑或石墨在粘合剂中。合适的导电背面胶层公开在美国专利5,108,463和5,137,452中,该专利在本文引用作为参考。
为了促进底涂层18和/或背面胶层24(如果有的话)的粘结,可能需要将这些层要贴敷于其上的表面改性。合适的表面改性包括电晕放电、紫外光曝光、电子束照射、火焰放电和折皱变形。
或者,虽然没有在附图中具体画出,磨料层14可以含有大量的磨粒分散在底涂层中。这种结构还可以在底涂层之上包含一个如上所述的超定型涂层。图2所示的结构和磨粒分散在底涂层中的那种结构都是在底涂层或第一粘合剂中含有磨料颗粒的磨料层实例。
根据本发明的涂敷磨料制品可以通过在预成型的衬材12上涂敷磨料层14来制备。为制备热熔底涂层,将各组分在合适的容器中于搅拌下混合,直到各组分彻底地熔融混合,最好是在对光化辐射不透明的容器中混合,混合温度应该高得足以使物质液化,以便使它们能有效地混合,而又不会受热降解(例如在120℃左右)。各组分可以同时加入或顺序加入,但是最好是先将含环氧物质和聚酯组分混合,接着加入含羟基物质,然后加入引发剂。
热熔底涂层应当在熔融相中相容。也就是说,各组分之间应当没有可见的粗相分离。底涂层可以在熔融混合后直接使用,也可以作为无溶剂体系包装在桶、筒或其它合适的容器中,最好是在避光下包装,直到准备使用。这样包装的底涂料可以使用卸桶器和类似装置输送到热熔涂布器系统。或者是,可以将本发明的热熔底涂层以棒、丸、小块、大块、枕形块或短条的形式输送到常规的批量热熔涂布器和分配器系统。
也可以将本发明的热熔底涂层作成未固化无载体的粘性压敏型粘结薄膜卷。这种薄膜适合用于将底涂层层压到磨料制品衬材上。最好是将这种粘性膜与一种防粘衬材(例如涂硅氧烷的牛皮纸)一起打卷,随后包装在对光化辐射不透明的袋里或其它容器中。
本发明的热熔底涂层可以用挤压、凹版印刷或涂布方法(例如用涂布模头、加热刮刀涂布器、辊涂器、帘式涂布器或反辊涂布器)敷加到磨料制品衬材上。在用上述的任何方法敷加时,底涂料宜在约100-125℃的温度下施用,优选约80-125℃对于使用J重量布料衬材和孔度类似的其它织物衬材的情形,涂布是一种理想的敷料方法。
热熔底涂层可以以自立式无载体的形式供应,它可以层压到衬材上,如有必要,在层压前将其冲切成预定的形状。选择层压的温度和压力,以便使衬材的损伤和底涂层的渗流物减至最少,其范围可以从室温到约120℃和约30-250磅/平方英寸。一种典型的方式是在室温和100磅/平方英寸下层压。对于使用高孔性的衬材,例如使用比标准的J重量布料更多孔的衬材的情形,层压是一种特别优选的敷料方法。
最好是用上述的任何一种方法将热熔底涂层敷加在磨料制品衬材上,一旦敷加上之后,立即暴露于能源之下以引发含环氧树脂的固化。据信这种含环氧的物质本身并与任意加入的含羟基物质一起,或许在某种程度上还与聚酯组分一起,发生固化或交联。
热熔底涂层在暴露于任何产能源之下时开始固化,并且在这之后继续一段时间。这种能量可以是电磁能(例如波长在光谱的紫外或可见区的辐射)、加速粒子(例如电子束辐射)或热能(例如加热或红外辐射)。此能量最好是光化辐射(即,波长在紫外或可见光谱区内的辐射)。合适的光化辐射源包括汞灯、氙灯、碳弧灯、钨丝灯、日光灯等。紫外辐射,尤其是中压汞弧灯的紫外辐射,最为优选。曝光时间可以从少于1秒到10分钟或更长(提供约1.0焦耳/平方厘米(J/cm2)的总曝光能),这取决于所涉及的反应物的数量及类型,能量来源,离能源的距离以及要固化的底涂层的厚度。
底涂层也可以通过电子束辐射来固化。所需的剂量一般是从小于1兆拉德到100兆拉德或更大。在指定的辐照能量下,固化速度会随引发剂数量的增加而增加。固化速度也随能量强度的增加而增加。
热熔底涂层中含有有延缓固化速度的聚醚多元醇则特别理想,因为延缓固化能使底涂层的压敏性质保留一段时间,足以使磨料颗粒在底涂层已暴露在能量作用下之后与其粘结(使用金属茂盐引发剂而不用聚醚多元醇,可以有类似的效果)。可以施加磨料一直到底涂层已充分固化,于是磨粒不再粘结,但是为了提高工业操作的速度,最好是尽可能快地施加磨粒,一般是在底涂层暴露于能源之下的几秒钟之内。因此可以理解,聚醚多元醇能为热熔底涂层提供一个间隔时间。也就是说,在底涂层已暴露于能量作用下之后的一段时间(间隔时间)里,对于要与之粘结的磨料颗粒它保持充分的粘性并且不固化。磨粒是用任何合适的方法投射到底涂层中,优选用静电涂布法。
利用热(例如在炉中)对底涂层进行后固化可以缩短达到完全固化的时间。后固化也会影响底涂层的物理性质,通常是合乎需要的。后固化的时间和温度随聚酯组分的玻璃化转变温度、引发剂的浓度、所受的能量状态等条件而变。后固化的条件可以从在约150℃下不到1分钟到较低温度下的较长时间。通常,后固化的条件是在约80℃下约2分钟。
在另一种制造方法里,将底涂层敷加到衬材上,然后将磨料颗粒投射到底涂层中,接着将底涂层暴露于能量作用之下。虽然此方法中为将底涂层固化所需的总能量与在加磨料颗粒之前先使底涂层受能量作用的方法中大致相同,但是最好是使用强度较小的能量作用较长的时间。在实施这种方法时一般不需要加热后固化。
如果磨料层由磨料颗粒在底涂层中的分散体构成,则配制一个含有磨粒和底涂层的磨料浆体,用辊涂、浸涂、刮涂等方法将其涂敷在衬材上。然后用上述方法将底涂层固化。
接着可以用各种方法,例如辊涂、喷涂或帘涂法,将定型涂层20以可流动的液体的形式施加在磨粒和底涂层上,随后用干燥、加热或者用电子束或紫外光辐射的方法固化。具体的固化方式可以随定型涂层的化学性质而变。任选采用的超定型涂层22可以按类似的方式涂敷和固化。
任选采用的背面胶层24可以许多常用涂布方法的任何一种(例如浸涂、辊涂、喷涂、Meyer棒、刮涂法、凹板印刷、热质转移、橡皮凸版印刷、网板印刷等)施加在衬材12上。
本发明的底涂层实现了各种高度理想性质的极好的平衡。作为无溶剂制剂,它们容易用常规的热熔体分配系统施加。因此,它们可以以很适合层压到衬材上的压敏性粘结薄膜的形式供应。包含的聚酯组分使底涂层具有压敏性,这有利于在它上面施加磨料颗粒。含有分子量和官能度合适的聚醚多元醇使本发明的底涂层在受到能量作用后有一个间隔时间,从而可以在底涂层已受到能量作用后向其中加入磨料颗粒。但是,这种热熔组合物固化后形成坚韧、耐久、自动粘合和交联的热固型底涂层。
参照以下非限制性实施例将会更全面地理解本发明,其中所有的份数均指重量。实施例中所用的缩与具有以下一览表中的定义。
DYNAPOL S1402 一种低结晶度的高分子量聚酯Huls America公司)
EPON 828 环氧当量约为185-192克/当量的双酚A环氧树脂(壳牌化学公司
EPON 1001F 环氧当量约为525-550克/当量的双酚A环氧树脂(壳牌化学公司
tBOX 乙二酸二叔丁酯,一种促进剂
CHDM 环己烷二甲醇,一种含羟基物质
VORANOL 230-238 羟基数为38的甘油和环氧丙烷的多羟基加成物(Dow化学公司
COM η6-[二甲苯(异构体混合物)]η5-环戊二烯基铁(1+)六氟锑酸盐,一种引发剂
AMOX 乙二酸二叔戊基酯,一种促进剂
TSA 三苯锍六氟锑酸盐,引发剂
BORDEN8505 脲醛树脂(Borden公司)
实施例1
实施例1的涂敷磨料制品包括一个已经润湿和拉伸、但是未经密封的J重量棉质衬材。为制备含DYNAPOL s1402(40.4份)、E-PON828(19.3份)。EPON1001F(29.9份)。CHDM(2.4份)、COM(1.0份)和AMOX(0.6份)的底涂层,将EPON828、EPON1001F和DYNAPOL S1402在合适的反应容器中于121℃下预热30分钟。然后加入CHDM,在121℃下混合3小时直到得到均匀的熔融混合物。将温度降至100℃,加入AMOX和COM,在100℃下搅拌1小时。
用连续式模涂法将底涂层于125℃下施加在衬材的前表面上,涂布量约为84克/平方米(g/m2)。底涂层(在衬材上)用一台UVXL-200/300/400瓦/英寸三挡D型紫外灯(Aetek International公司,Plainfield,Illinois)照射,紫外灯在200瓦/英寸的一挡工作,卷材的进料速度为0.10米/秒,于是总曝光能量约为50-60毫焦耳/cm2。在底涂层经受紫外辐射后,立即将80号的熔融氧化铝磨料颗粒以327g/m2的加入量加入到底涂层中。然后将所形成的产品在80℃下后固化30分钟。
将含有BORDEN8405(6500份)、长石(2100份)、氯化铝(452份,10%固体在水中)和水(948份)的60%固体含量的定型涂层辊涂在磨料颗粒之上,湿涂布量约为159g/m2。将得到的制品在66℃下加热45分钟,然后在试验前将它弯曲。
实施例2
实施例2根据实施例1中所述步骤制备,但是以约126g/m2的涂布量涂敷底涂层。
对照实施例1和2
还提供了两个使用市售涂敷磨料制品的对照实施例。对照实施例(C.E)1是一个80号3M211 ELEK-TRO-OUT涂敷磨料制品,它有一个J重量级布料衬材,3M公司销售。对照实施例2是一个有J重量级布料衬材的80号3M 311T BLUE GRIT涂敷磨料制品,也可由3M公司买到。
实施例3
一个底涂层中含有DYNAPOL S1402(40.0份)、EPON828(15.0份)、EPON1001F(29.0份)、VORANOL230-238(15.0份)和TSA(1.0份),制备时将这些物质在合适的容器中于121℃下掺混15分钟,直到各组分熔融混合,接着再混合5分钟。将此底涂层在125℃下用加热刮刀以约49g/m2的涂布量涂敷在与实施例1中所用的同样衬材上。以约209g/m2的重量将120号氧化铝磨粒滴涂在底涂层内。所形成的产品立即在氮环境中以无机物一面暴露在F15T8350BL(Sylvania公司)低强度紫外辐射灯下(以0.51厘米/秒的卷材进料速度在1000毫焦耳/cm2下10分钟)。然后将实施例1的定型涂层以约109g/m2的湿涂布量辊涂在磨料颗粒之上。
实施例4
根据实施例3的步骤制备实施例4,但是以约123g/m2的涂布量涂敷底涂层。实施例3和4表明,底涂层可以在施加磨料颗粒之后进行能量固化。
对照实施例3
对照实施例3是有J重量级多用布衬材的120号3M311T BLUE GRIT涂敷磨料制品,可自3M公司购得。
实施例5
根据实施例1所述的步骤制备底涂层,在125℃下用加热刮刀式涂布器涂敷在两个约102μm厚的防粘衬里之间,涂布量约为84g/m2,从而形成一个自立的粘性压敏型粘结膜。除掉一个防粘衬里,将粘结膜的外露表面在室温下(约20-22℃)以约690千帕的压力层压在棉质衬材上。底涂层象实施例1中一样辐射。然后用磨料颗粒涂敷所形成的制品,加热进行后固化,形成定型涂层,加热并弯曲,全按实施例1中所述。实施例5表明,在本发明的涂敷磨料制品中使用的底涂层可以作成自立式的粘性压敏型粘结薄膜,它可以层压在多孔的布衬材上。
根据以下的某些或全部步骤,试验实施例1到5和对照实施例1到3。
试验步骤
90°剥离试验
为了测定衬材和底涂层之间的粘结力,将几个实施例和对照实施例的涂敷磨料制品改制成宽约8cm、长约25cm的样品。将一块木反(长17.78cm、宽7.62cm、厚0.64cm)的一半长度涂上3M公司销售的JET-MELT3779-PG粘结剂。在涂敷磨料制品的全部宽度、但是仅仅头15cm长度上,用同样的粘结剂涂在有磨粒的一面。将制品的带磨粒和粘结剂的一面贴在木板的有粘结剂的一面上,涂敷磨料制品不带粘结剂的那10cm部分悬在木板的外面。施加压力使木板和制品紧密粘结。构成试验装置,其结构方式要保证试验时的分离发生在涂敷磨料制品的各层之间,而不是在涂敷磨料制品和木板之间。
随后沿直线划开磨料制品,以便使其宽度减小到5.1cm。将所形成的涂敷磨料制品/木板组合件水平地装在一台SINTECH拉力试验机的下钳口上,约1cm的涂敷磨料制品外悬部分装在上钳口上。两个钳口之间的距离为12.7cm,分离速度为0.5cm/sec,将涂敷磨料制品以90°角从木板上拉开,从而使底涂层与布衬材分离。以每厘米制品宽度的千克数(kg/cm)记录分离力,此数值越大表示底涂层与布衬材之间的粘结越好。分离力以至少为1.8kg/cm为佳,至少为2kg/cm则更好。结果列在下面的表1中。
园片试验
用园片试验评价涂敷磨料制品研磨聚合物加工件的能力,结果示于下面的表1中。更具体地说,将实施例1和2和对照实施例1和2的涂敷磨料制品冲切成10.2cm直径的园片,用压敏型粘结剂将它们粘在泡沫塑料支承热上。将涂敷磨料园片和泡沫塑料支承垫装在一台Schiefer试验装置上,在4.5kg的负荷下干磨一个聚甲基丙烯酸甲酯加工件500转。加工件是一个有贯穿中心部分的开口的园片。园片的外径为10.2cm,内径为5.1cm。称量磨下的聚全物克数(g)、测量Ra(用微英寸10-6英寸)表示的划痕深度的算术平均值)以确定所磨的加工件的表面光洁度。磨下的聚合物的重量应该至少约1.3克。
摇摆器转鼓试验
使用摇摆器转鼓试验评价涂敷磨料制品研磨金属加工件的能力。更具体地说,将实施例3和4及对照实施例1和2的涂敷磨料制品改制成10.2cm宽、15.2cm长的薄片,将它们装在摇摆器转筒试验机的园柱形转鼓上,试验机以每分钟约60个冲程的速度前后振动(摇摆,一个完整的前后循环等于一个冲程)。相对于静止的宽1.3cm、长15.2cm、厚1.3cm的3008F型铝加工件的这种振动运动在涂敷的磨料制品上磨出一个约1.3cm宽、14.0cm长的轨迹。施加在加工件的力为2.7kg。测量磨下的铝的克数,结果列在下面的表1中。表中在斜线后的数字表示试验片所经受的循环数目。
表 1
实施例 | 90°剥离力(kg/cm) | 磨下的材料(g) | Ra10-6英寸 | |
园片试验 | 摇摆式转鼓试验 | |||
12对照例1对照例234对照例35 | 2.02.0未试验2.02.32.9未试验2.1 | 1.371.281.311.32未试验未试验未试验1.64 | 未试验0.17/62未试验0.98/4020.31/1000.31/1000.32/1000.83/100 | 979.0113105未试验””” |
表1的数据表明,与对照实施例1和2相比,实施例1和2在剥离力和园片试验方面性能相近,同时光洁度略高,而且不需要衬材上有饱和涂层或类似物。与对照实施例3相比,实施例3和4表明即使衬材上没有饱和涂层或类似涂层,这些涂敷磨料制品的性能仍与市售的涂敷磨料制品相近。
在上述说明书和附图的范围之内可以作许多修改和变动而不背离在所附权利要求中限定的本发明。
Claims (15)
1、一种由衬材、衬材上的第一粘合剂和在第一粘合剂中的大量磨料颗粒构成的涂敷磨料制品,其中第一粘合剂是经过能量固化成交联的涂层的热熔压敏型粘合剂。
2、根据权利要求1的涂敷磨料制品,其中在第一粘合剂和磨料颗粒之上还有第二粘合剂。
3、制备权利要求1的涂敷磨料制品的方法,其中包括以下步骤:
(a)构成一个衬材;
(b)在衬材上敷加可以能量固化的热熔压敏粘结型第一粘合剂;
(c)使第一粘合剂暴露在产能源之下,以引发第一粘合剂固化;
(d)在第一粘合剂中沉积大量磨料颗粒;和
(e)使第一粘合剂固化成其中带有磨料颗粒的交联涂层。
4、根据权利要求1、2或3中任何一个的涂敷磨料制品,其中衬材是多孔的布、纺织品或织物材料。
5、根据权利要求1、2或3中任何一个的涂敷磨料制品,其中第一粘合剂含有含环氧物质、聚酯组分和用于第一粘合剂能量固化的有效数量的引发剂。
6、根据权利要求5的涂敷磨料制品,其中第一粘合剂含有:
(a)约2到95份含环氧物质;
(b)相应地,约98到5份聚酯组分,其中(a)+(b)之和等于100份;
(c)用于第一粘合剂能量固化的有效数量的引发剂;
(d)一种任意加入的含羟基物质,其羟基官能度至少为1。
7、根据权利要求6的第一粘合剂,其中聚酯组分的数均分子量约为7500至20000。
8、根据权利要求7的第一粘合剂,其中聚酯组分的数均分子量约为15000至30000。
9、根据权利要求5的第一粘合剂,其中聚酯组分是(a)二羧酸和(b)有2-12个碳原子的二元醇的反应产物,该二羧酸选自含4-12个碳原子的饱和脂族二羧酸(及其二酯衍生物)和含8-15个碳原子的芳族二羧酸(及其二酯衍生物)。
10、根据权利要求6的第一粘合剂,其中有作为含羟基物质存在的聚亚氧烷基多元醇。
11、根据权利要求10的第一粘合剂,其中聚亚氧烷基多元醇选自聚氧乙烯二醇、聚氧乙烯三醇、聚氧丙烯二醇和聚氧丙烯三醇。
12、根据权利要求6的第一粘合剂,其中第一粘合剂含有2-80份含环氧物质和相应地98-20份聚酯组分。
13、根据权利要求12的第一粘合剂,其中第一粘合剂含有2-60份含环氧物质和相应地98-40份聚酯组分。
14、一种制备权利要求3的涂敷磨料制品的方法,其中在第一粘合剂已受到产能源作用之后将磨料颗粒沉积在第一粘合剂中。
15、一种制备权利要求3的涂敷磨料制品的方法,其中在第一粘合剂受能源作用之前将磨料颗粒沉积在第一粘合剂中。
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EP0276716A3 (en) * | 1987-01-30 | 1989-07-26 | General Electric Company | Uv curable epoxy resin compositions with delayed cure |
US4799939A (en) * | 1987-02-26 | 1989-01-24 | Minnesota Mining And Manufacturing Company | Erodable agglomerates and abrasive products containing the same |
US4997717A (en) * | 1987-03-27 | 1991-03-05 | Ciba-Geigy Corporation | Photocurable abrasives |
JPH0628269B2 (ja) * | 1987-07-15 | 1994-04-13 | 株式会社巴川製紙所 | ダイボンデイング用接着テ−プ |
DE3727847A1 (de) * | 1987-08-20 | 1989-03-02 | Fuller H B Co | Schmelzklebstoff und verfahren zu seiner herstellung und verarbeitung |
US4920182A (en) * | 1987-12-18 | 1990-04-24 | Ciba-Geigy Corporation | Epoxy resin compositions containing polyester flexibilizer and metallocene complex initiator |
JPH01268776A (ja) * | 1988-04-21 | 1989-10-26 | Unitika Ltd | ホツトメルト接着剤組成物 |
US4927431A (en) * | 1988-09-08 | 1990-05-22 | Minnesota Mining And Manufacturing Company | Binder for coated abrasives |
IT1227361B (it) * | 1988-11-18 | 1991-04-08 | Enichem Sintesi | Composizione di hot melt reattivo. |
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US4903440A (en) * | 1988-11-23 | 1990-02-27 | Minnesota Mining And Manufacturing Company | Abrasive product having binder comprising an aminoplast resin |
JPH02239447A (ja) * | 1989-03-10 | 1990-09-21 | Ricoh Co Ltd | 光磁気記録媒体 |
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FR2664284B1 (fr) * | 1990-07-05 | 1994-07-08 | Ceca Sa | Resines tackifiantes modifiees et produits assimiles pour adhesifs thermofusibles reticulables par l'humidite; adhesifs thermofusibles les incorporant et leurs applications. |
EP0552190B1 (en) * | 1990-10-09 | 1996-12-18 | Minnesota Mining And Manufacturing Company | Coated abrasive containing erodable agglomerates |
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CA2108260A1 (en) * | 1991-05-16 | 1992-11-17 | Kam Chu Wu | Epoxide-based adhesive |
US5203884A (en) * | 1992-06-04 | 1993-04-20 | Minnesota Mining And Manufacturing Company | Abrasive article having vanadium oxide incorporated therein |
US5286541A (en) * | 1992-09-10 | 1994-02-15 | Norton Company | Coated abrasive having combination backing member |
-
1993
- 1993-04-15 US US08/047,861 patent/US5436063A/en not_active Expired - Lifetime
-
1994
- 1994-03-10 CA CA002118766A patent/CA2118766C/en not_active Expired - Lifetime
- 1994-03-29 ZA ZA942227A patent/ZA942227B/xx unknown
- 1994-04-13 KR KR1019940007710A patent/KR100332249B1/ko not_active IP Right Cessation
- 1994-04-14 CN CN94104609A patent/CN1072091C/zh not_active Expired - Lifetime
- 1994-04-14 DE DE69426469T patent/DE69426469T2/de not_active Expired - Lifetime
- 1994-04-14 JP JP07578694A patent/JP3943143B2/ja not_active Expired - Fee Related
- 1994-04-14 EP EP94105787A patent/EP0620083B1/en not_active Expired - Lifetime
- 1994-04-14 AT AT94105787T patent/ATE198287T1/de not_active IP Right Cessation
-
1995
- 1995-06-01 US US08/457,390 patent/US5582672A/en not_active Expired - Lifetime
-
1996
- 1996-06-25 US US08/670,052 patent/US5834109A/en not_active Expired - Lifetime
- 1996-07-03 US US08/675,136 patent/US5776290A/en not_active Expired - Lifetime
-
2007
- 2007-03-05 JP JP2007054447A patent/JP2007181918A/ja not_active Withdrawn
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CN101808781B (zh) * | 2007-08-03 | 2014-10-22 | 圣戈班磨料磨具有限公司 | 具有助黏附层的磨料物品 |
CN102212969A (zh) * | 2010-04-06 | 2011-10-12 | 厚生股份有限公司 | 高丹尼防水透湿织物的加工方法 |
CN102009038A (zh) * | 2010-09-17 | 2011-04-13 | 淄博理研泰山涂附磨具有限公司 | 一种涂附磨具的热熔型超涂层涂附方法 |
CN110869206A (zh) * | 2017-07-11 | 2020-03-06 | 3M创新有限公司 | 包括可适形涂层的磨料制品和由此形成的抛光系统 |
CN110869166A (zh) * | 2017-07-11 | 2020-03-06 | 3M创新有限公司 | 包括适形涂层的磨料制品和由其形成的抛光系统 |
TWI803498B (zh) * | 2017-07-11 | 2023-06-01 | 美商3M新設資產公司 | 包括可適形塗層之磨料物品及來自其之拋光系統 |
CN107718729A (zh) * | 2017-11-10 | 2018-02-23 | 江苏瑞和磨料磨具有限公司 | 一种柔软耐水强力磨砂布 |
CN108637925A (zh) * | 2018-04-24 | 2018-10-12 | 安徽禾臣新材料有限公司 | 一种精密光学器件抛光用阻尼布及其制备方法 |
CN108637925B (zh) * | 2018-04-24 | 2020-08-04 | 安徽禾臣新材料有限公司 | 一种精密光学器件抛光用阻尼布及其制备方法 |
CN112092388A (zh) * | 2020-09-30 | 2020-12-18 | 芜湖金三氏数控科技有限公司经开区分公司 | 一种pvb膜钨丝排布设备 |
CN115247032A (zh) * | 2022-04-06 | 2022-10-28 | 上海固柯胶带科技有限公司 | 一种晶圆减薄用高效研磨胶带及其制备方法 |
CN115247032B (zh) * | 2022-04-06 | 2023-10-17 | 上海固柯胶带科技有限公司 | 一种晶圆减薄用高效研磨胶带及其制备方法 |
Also Published As
Publication number | Publication date |
---|---|
DE69426469D1 (de) | 2001-02-01 |
KR100332249B1 (ko) | 2002-11-30 |
JPH071344A (ja) | 1995-01-06 |
US5834109A (en) | 1998-11-10 |
EP0620083A1 (en) | 1994-10-19 |
CA2118766A1 (en) | 1994-10-16 |
US5776290A (en) | 1998-07-07 |
CA2118766C (en) | 2005-02-01 |
US5582672A (en) | 1996-12-10 |
JP2007181918A (ja) | 2007-07-19 |
ATE198287T1 (de) | 2001-01-15 |
US5436063A (en) | 1995-07-25 |
ZA942227B (en) | 1995-09-29 |
EP0620083B1 (en) | 2000-12-27 |
DE69426469T2 (de) | 2001-09-20 |
CN1072091C (zh) | 2001-10-03 |
JP3943143B2 (ja) | 2007-07-11 |
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