CN102123768B - 基于聚氨酯的网球的制备方法 - Google Patents
基于聚氨酯的网球的制备方法 Download PDFInfo
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- CN102123768B CN102123768B CN2009801302167A CN200980130216A CN102123768B CN 102123768 B CN102123768 B CN 102123768B CN 2009801302167 A CN2009801302167 A CN 2009801302167A CN 200980130216 A CN200980130216 A CN 200980130216A CN 102123768 B CN102123768 B CN 102123768B
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Abstract
本发明涉及一种用于制备网球的泡沫聚氨酯,所述泡沫聚氨酯通过将以下组分混合得到一种反应混合物,并使所述反应混合物完成反应而获得:a)有机多异氰酸酯,b)多羟基化合物,c)如果合适,聚合物多元醇,d)发泡剂,e)催化剂,和如果合适,f)助剂和添加剂;所述b)多羟基化合物包含:b1)相对高分子量多羟基化合物,其平均OH官能度<2.5、摩尔质量为450-12 000g/mol且具有大于50%比例的伯羟基,并选自聚醚多元醇、聚酯多元醇和聚碳酸酯多元醇;和b2)低分子量二元醇,其摩尔质量为52-400g/mol;b3)如果合适,低分子量交联剂,其含有至少3个对异氰酸酯基团有反应活性的基团;其中组分b3)基于组分b)计的比例为0至5重量%,其中组分b2)基于组分b)计的比例为4至20重量%。
Description
技术领域
本发明涉及制备网球用泡沫聚氨酯。
背景技术
国际网球联合会(ITF)的网球规则规定了网球的精确规格。网球必须具有确定的尺寸、确定的重量、确定的回弹性和确定的受力-位移特性。例如,重量必须为56.7至58.5g,直径必须为6.35cm至6.67cm,当从254cm的高度落在水平硬质表面如混凝土上时,网球的回弹高度必须为134.6至147.3cm。
在球的周围有一层由羊毛和尼龙的混合物构成的结实的粘着毛毡层(felt layer)。对于每个球,将两个宽哑铃形毛毡片——在其反面涂有热熔粘合剂——粘结在球的橡胶球胆上并干燥。最后蒸汽处理使毛毡更膨松。位于毛毡下的橡胶球胆——也称为球芯——由包含某些添加剂(氧化铝、石英、硫、氧化锌和碳酸镁等)的天然橡胶构成。其以线材形式的均匀混合物挤出,并切成网球需要的部分。在模具中将其压缩得到半球形壳并硫化。为制备所谓的压力球(pressurized ball),将橡胶半壳的边缘粗化,然后用硫化溶液涂覆,并用硝酸钠和氯化铵构成的溶液涂覆橡胶半壳的内部。两个半壳通过硫化彼此结合,随之通过盐的分解和由此发生的氮气的释放在球内产生需要的超级大气压。在一个变形方法中,在超级大气压下结合两个半芯,随之在球芯中充入压缩气体(氮气)。
锦标赛用球的内压为1.6至2.2巴。气体会随时间逸出,从而弹力降低。为防止气体在比赛前逸出,球在具有相同压力的包装中出售,以使包装中的压力平衡。然而,气体会在使用中逸出:专业级别的1至2轮比赛中或在业余级别比赛的数周之后,导致球不能使用,并失去需要的弹力。
DE-A2844193公开了一种制备适用于网球运动的球的方法,该方法通过使用机械方法由含有基于聚醚的聚氨酯或基于聚酯的聚氨酯的泡沫制备所述球而进行。这种泡沫的密度为约160kg/m3。回弹性相当于常规网球的值。该方法中使用的泡沫材料的构成详细信息给出较少。所述全部信息只是,其有利地包括聚氨酯,优选基于聚醚的聚氨酯。
DE-A2639749涉及棒球比赛设备,还涉及适用于这种比赛的、由柔性材料构成的球。提及的合适柔性材料有合成柔性泡沫、柔性聚氨酯泡沫和廉价柔性复合泡沫、以及柔性天然橡胶泡沫。所述泡沫的密度要低于0.35kg/dm3,其冲击回弹性为40%至60%。
GB2008954涉及由基于聚醚或聚酯的聚氨酯泡沫构成的实心网球,其密度为30至400kg/m3,断裂伸长率为18至300%,优选75至300%,Shore-A硬度为70至75。没有公开聚氨酯泡沫的精确构成。
发明内容
本发明的一个目的是提供一种适用于制备网球的聚氨酯组合物,从而得到具有满足网球需要的回弹性和硬度的泡沫聚氨酯。所述泡沫聚氨酯特别是意在得到压力-位移(pressure-displacement)特性与常规网球相当的网球。
该目的通过如下的用于制备网球的泡沫聚氨酯实现,所述泡沫聚氨酯通过将以下组分混合得到一种反应混合物,并使所述反应混合物完成反应而获得:
a)有机多异氰酸酯,
b)多羟基化合物,包含
b1)相对高分子量多羟基化合物,其平均OH官能度≤2.5、摩尔质量为450至12000g/mol且具有大于50%比例的伯羟基,其选自聚醚多元醇、聚酯多元醇和聚碳酸酯多元醇,和
b2)低分子量二元醇,其摩尔质量为52至400g/mol、优选52至280g/mol,其中组分b2)在组分b)中的含量为4至20重量%,
b3)低分子量交联剂,其含有至少3个对异氰酸酯基团有反应活性的基团,其中组分b3)在组分b)中的含量为0至5重量%,
c)如果合适,聚合物多元醇,
d)发泡剂,
e)催化剂,和如果合适,
f)助剂和添加剂。
该目的还通过包含所述泡沫聚氨酯的网球实现。
该目的还通过包含组分a)至f)的组合物以及其用于制备网球的用途实现。
具有网球需要的回弹性和耐压强度的聚氨酯泡沫可通过使用包含相对高分子量多羟基化合物b1)和称之为增链剂的低分子量二元醇b2)的混合物得到。例如,根据附图的压力-位移特性,使用本发明组合物得到的网球的耐压强度对于38.5%的形变而言为300至400N,且回弹性为45至65%,优选50至60%。
附图说明
图1是使用本发明的聚氨酯组合物制备的网球以及参照的网球的压力-位移特性图。
具体实施方式
多异氰酸酯a)包含现有技术中已知的脂族、脂环族和芳香族双官能或多官能的异氰酸酯(成分a-1),及其任意所需混合物。实例有二苯甲烷4,4’-二异氰酸酯、二苯甲烷2,4’-二异氰酸酯、含有单体二苯甲烷二异氰酸酯和二苯甲烷二异氰酸酯多核同系物(聚合物MDI)的混合物、四亚甲基二异氰酸酯、六亚甲基二异氰酸酯(HDI)、异佛尔酮二异氰酸酯(IPDI)、甲苯2,4-二异氰酸酯或甲苯2,6-二异氰酸酯(TDI),或所述异氰酸酯的混合物。
优选使用4,4’-MDI。优选使用的4,4’-MDI可包含0至20重量%的2,4’-MDI和少量——最高达约10重量%——的脲基甲酸酯改性的或脲酮亚胺改性的多异氰酸酯。也可使用少量的聚亚苯基聚亚甲基多异氰酸酯(聚合物MDI)。聚合物MDI的总量不应超过所用异氰酸酯a)的5重量%。
多异氰酸酯组分a)优选以多异氰酸酯预聚物的形式使用。这些多异氰酸酯预聚物可通过使上述多异氰酸酯(a-1)与多元醇(a-2)在例如30至100℃的温度、优选约80℃下反应生成所述预聚物而获得。优选使用4,4’-MDI连同脲酮亚胺改性的MDI和基于聚醚的市售多元醇,例如包括环氧乙烷和/或环氧丙烷、或聚四氢呋喃(PTHF),或和聚酯(例如基于己二酸的那些)或和聚碳酸酯醇(polycarbonatole)(例如欧洲专利申请EP07101407.0中所述)制备所述预聚物。特别优选使用基于聚四氢呋喃的预聚物。
多元醇(a-2)是本领域技术人员已知的,并描述于例如“Kunststoffhandbuch,Band7,Polyurethane[Plastics handbook,volume7,Polyurethanes]”,Carl Hanser Verlag,3rd edition,1991,chapter3.1中。
基于醚的预聚物优选通过使多异氰酸酯(a-1)——特别优选4,4’-MDI——与二羟基和三羟基聚氧丙烯多元醇和/或聚氧丙烯聚氧乙烯多元醇反应而获得。其多数通过使环氧丙烷单独地或以与环氧乙烷的混合物或嵌段的形式与H-官能团(特别是OH-官能团)启动物质发生熟知的碱(KOH)催化加成反应而制备。使用的启动物质的实例有水、乙二醇或丙二醇及其低聚物、甘油或三羟甲基丙烷。多金属氰化物——所谓的DMC催化剂——也可用作催化剂。路易斯酸如三氟化硼也可用作催化剂。优选使用的组分(a-2)包含以下在b1)中描述的聚醚。还可伴随使用以下在b2)中描述的增链剂和以下在b3)中描述的交联剂。
使用环氧乙烷/环氧丙烷混合物时,基于环氧烷的总量计,环氧乙烷优选以10-50重量%的量使用。环氧烷的纳入此处可通过嵌段或以无规混合物形式实现。特别优选纳入环氧乙烷末端嵌段(“EO末端”)以提高较具反应活性的末端伯OH基团的含量。所述多元醇(a-2)的数均摩尔质量优选为400至12000g/mol,特别优选500至8000g/mol,特别是600至6000g/mol。
如果合适,在所述异氰酸酯预聚物的制备过程中向所述多元醇中加入常规增链剂或交联剂。此类物质描述于以下b2)和b3)中。特别优选使用双丙甘醇或三丙二醇作增链剂。
本发明组合物包含多羟基化合物作组分b),其包含
b1)相对高分子量多羟基化合物,其平均OH官能度≤2.5、摩尔质量为450至12000g/mol且具有大于50%比例的伯羟基,其选自聚醚多元醇、聚酯多元醇和聚碳酸酯多元醇,和
b2)低分子量二元醇,其摩尔质量为52至400g/mol,和
b3)如果合适,低分子量交联剂,其含有至少3个对异氰酸酯基团有反应活性的基团。
相对高分子量多羟基化合物b1)选自聚醚多元醇、聚酯多元醇和聚碳酸酯多元醇,优选聚醚多元醇、聚酯多元醇、及其混合物,特别优选聚醚多元醇,特别是聚四氢呋喃多元醇。
合适的聚醚多元醇b1)通过已知方法由一种或多种在其亚烷基基团中具有2至4个碳原子的环氧烷制备,例如通过使用碱金属氢氧化物或碱金属醇盐作为催化剂并加入至少一种启动分子进行的阴离子聚合,或通过使用路易斯酸作为催化剂进行的阳离子聚合;所述启动分子含有2至3个对异氰酸酯基团有反应性的氢原子;所述路易斯酸例如五氯化锑和氟化硼***合物。合适的环氧烷的实例有四氢呋喃、1,3-环氧丙烷、1,2-环氧丁烷或2,3-环氧丁烷以及优选的四氢呋喃、环氧乙烷和1,2-环氧丙烷。可使用的其他催化剂有多金属氰化物——所谓的DMC催化剂。所述环氧烷可单独使用,或者交替地相继使用或以混合物的形式使用。优选由1,2-环氧丙烷和环氧乙烷构成的混合物,其中10至50%的量的环氧乙烷用作环氧乙烷末端(“EO末端”)以使形成的多元醇总体含有70%以上的末端伯OH基团。例如,在聚四氢呋喃多元醇情况下,使四氢呋喃阳离子开环并聚合。
可使用的启动分子有水和二元醇和三元醇,例如乙二醇、1,2-丙二醇和1,3-丙二醇、二甘醇、双丙甘醇、1,4-丁二醇、甘油或三羟甲基丙烷,优选乙二醇、1,2-丙二醇和1,3-丙二醇、二甘醇、双丙甘醇、三丙二醇和1,4-丁二醇。
聚醚多元醇b1)的平均OH官能度一般为1.5至3、优选1.6至2.9、特别优选1.7至2.7、特别是约2,摩尔质量为1000至12000g/mol、优选1400至8000g/mol、特别优选1700至6000g/mol。
优选的聚醚多元醇b1)有聚氧丙烯聚氧乙烯多元醇、聚四氢呋喃多元醇、及其混合物。
所述聚氧丙烯聚氧乙烯多元醇总体包含70至95重量%的环氧丙烷单元和5至30重量%的环氧乙烷单元。其伯OH基团含量为至少50%,优选至少70%。
特别优选使用聚四氢呋喃多元醇作聚醚多元醇b1),且特别优选以与至少一种另外的聚醚多元醇的混合物的形式使用。此处聚四氢呋喃的数均分子量一般为550至4000g/mol,优选750至3000g/mol,特别优选800至2500g/mol,特别是约2000g/mol。
优选的另外的聚醚多元醇有已使用一种上述二元醇和三元醇——特别是使用乙二醇、1,2-丙二醇和1,3-丙二醇、二甘醇、双丙甘醇和三丙二醇——起始的聚氧丙烯聚氧乙烯多元醇,其伯OH基团的比例至少为70%,且数均摩尔质量为1000至12000g/mol、优选1400至8000g/mol、特别优选1700至6000g/mol。另外的聚醚多元醇的存在可取得极精确的需要的回弹性,同时保持所述压力-位移特性。
特别优选的聚醚多元醇b1)为由
b11)50至90重量%的聚四氢呋喃多元醇和
b12)10至50重量%的另外的聚醚多元醇
构成的混合物。
合适的聚酯多元醇一般由具有2至12个碳原子的有机二元羧酸(优选具有4至6个碳原子的脂肪族二元羧酸)和含有2至12个碳原子(优选2至6个碳原子)的多元醇(优选二元醇)制备。可用的二元羧酸的实例有:琥珀酸、戊二酸、己二酸、辛二酸、壬二酸、癸二酸、马来酸、富马酸、邻苯二甲酸、间苯二甲酸和对苯二甲酸。此处所述二元羧酸可单独使用或彼此混合使用。除了游离的二元羧酸之外,还可以使用相应的二元羧酸衍生物,例如具有1至4个碳原子的醇的二羧酸酯,或二羧酸酐。优选使用数量比例为例如20至35:35至50:20至32重量份的琥珀酸、戊二酸和己二酸的二元羧酸混合物,特别是己二酸。二元醇和多元醇——特别是二元醇——的实例有:乙二醇、二甘醇、1,2-丙二醇或1,3-丙二醇、双丙甘醇、1,4-丁二醇、1,5-戊二醇、1,6-己二醇、1,10-癸二醇、甘油和三羟甲基丙烷。优选使用乙二醇、二甘醇、1,4-丁二醇、1,5-戊二醇和1,6-己二醇。也可使用由内酯(如ε-己内酯)或羟基羧酸(如ω-羟基己酸)衍生的聚酯多元醇。
为制备所述聚酯多元醇,可将所述有机——例如芳香族和优选脂肪族——多元羧酸和/或其衍生物和多元醇在不存在催化剂的条件下、或优选在存在酯化催化剂的条件下缩聚至降至所需的酸值,所述酸值优选小于10,特别优选小于2,所述缩聚有利地在由惰性气体例如特别是氮气、一氧化碳、氦气、氩气等构成的气氛中进行,在150至250℃、优选180至220℃的温度下在熔体中进行,并且如果合适减压进行。在一个优选实施方案中,所述酯化混合物在大气压力下在上述温度下缩聚至酸值达到80至30、优选40至30,然后在小于500mbar的压力下、优选50-150mbar的压力下缩聚。可用的酯化催化剂的实例有金属、金属氧化物或金属盐形式的铁催化剂、镉催化剂、钴催化剂、铅催化剂、锌催化剂、锑催化剂、镁催化剂、钛催化剂和锡催化剂。然而,所述缩聚也可以在液相中在稀释剂和/或共沸剂的存在下进行,所述共沸剂例如苯、甲苯、二甲苯或氯苯,以共沸蒸馏除去缩合的水。为制备所述聚酯多元醇,所述有机多元羧酸和/或其衍生物与多元醇有利地以1:1-1.8、优选1:1.05-1.2的摩尔比进行缩聚。
形成的聚酯多元醇的平均OH官能度优选为2.0至2.5,摩尔质量为480至5000g/mol、优选1000至4500g/mol、特别是1600至4000g/mol。
所述相对高分子量的多羟基化合物b1)的平均OH官能度小于2.5。所述相对高分子量的多羟基化合物的平均OH官能度优选小于2.2。当此处使用聚四氢呋喃多元醇时,基于所述相对高分子量的多羟基化合物b1)的总重量计,二元醇的比例大于50重量%、特别优选大于80重量%、特别是100重量%。
合适的低分子量二元醇b2)有乙二醇、二甘醇、1,2-丙二醇或1,3-丙二醇、双丙甘醇、三丙二醇、1,4-丁二醇、1,5-戊二醇、1,6-己二醇和1,10-癸二醇,优选乙二醇和1,4-丁二醇、二甘醇和1,6-己二醇,特别优选乙二醇和1,4-丁二醇。
还可使用两种或更多种所述低分子量二元醇b2)的混合物。在本发明的一个具体实施方案中,使用乙二醇和1,4-丁二醇的混合物。
此处所述低分子量二元醇b2)在组分b)中的比例为4至20重量%、优选4.5至15重量%、特别是5至9重量%。
合适的低分子量交联剂b3)优选为三元醇或多羟基多元醇——其摩尔质量一般为92至800g/mol、优选92至600g/mol。实例有甘油、三羟甲基丙烷、季戊四醇、山梨醇和蔗糖——,以及一般每分子含有平均3至20个环氧烷单元(环氧乙烷和/或环氧丙烷)的它们的烷氧基化物。
聚合物多元醇可伴随用作组分c)。聚合物多元醇一般是已知的并可市售获得。聚合物多元醇通过以下方式制备:使用一种自由基引发剂(通常为偶氮化合物或过氧化合物)使单体(优选丙烯腈、苯乙烯和如果合适其他单体)、大分子单体,以及如果合适缓和剂(moderator)在作为连续相的聚醚醇或聚酯醇中进行自由基聚合。作为连续相从而作为分散介质的聚醚醇或聚酯醇也常被称为载体多元醇。以下专利说明书提供了此处聚合物多元醇的制备实例:US4,568,705、US5,830,944、EP0163188、EP0365986、EP0439755、EP0664306、EP0622384、EP0894812和WO00/59971。该一般方法为丙烯腈、苯乙烯、或优选地苯乙烯和丙烯腈的混合物——例如重量比为90:10至10:90、优选70:30至30:70——的原位聚合。
可使用的载体多元醇为在b1)中描述的所有多元醇。大分子单体也称为稳定剂,是分子量≥1000g/mol的线性或支链聚醚醇,其大多含有末端的反应性烯键式不饱和基团。所述烯键式不饱和基团可通过与以下物质反应而连接至现有的多元醇:羧酸如丙烯酸,酰卤如丙烯酰氯,羧酸酐如马来酸酐,富马酸,丙烯酸酯衍生物和甲基丙烯酸酯衍生物,或烯键式不饱和环氧化物如1-乙烯基环己烯-3,4-环氧化物、1-丁二烯单氧化物、乙烯基缩水甘油醚、甲基丙烯酸缩水甘油酯和烯丙基缩水甘油醚,或者异氰酸酯衍生物如3-异丙烯基-1,1-二甲基苯甲基异氰酸酯或异氰酸乙酯基甲基丙烯酸酯。另一种方法是使用具有羟基和烯键式不饱和度的启动分子通过环氧丙烷和环氧乙烷的烷氧基化而制备多元醇。此类大分子单体的实例描述于以下文献中:US4,390,645、US5,364,906、EP0,461,800、US4,997,857、US5,358,984、US5,990,232、WO01/04178和US6,013,731。
在自由基聚合反应中,所述大分子单体也伴随纳入聚合物链中。产物为具有聚醚嵌段和聚丙烯腈-苯乙烯嵌段的共聚物,所述共聚物起连续相和分散相之间界面处的增容剂的作用,并抑制聚合物多元醇颗粒的集聚。大分子单体的比例可最高达超过90重量%、通常为1至60重量%、优选1至40重量%、特别优选1至15重量%,各自基于用于制备聚合物多元醇的单体的总重量计。
聚合物多元醇优选通过使用——作为载体多元醇——主要含有伯OH基团且数均摩尔质量为1000至12000g/mol——优选1400至8000g/mol、特别优选1700至6000g/mol——的二羟基或三羟基聚醚多元醇制备。
优选使用的聚合物多元醇有基于聚氧丙烯-聚氧乙烯多元醇或聚四氢呋喃多元醇(PTHF)制备的那些,且通常其数均摩尔质量为500至12000g/mol、优选750至8000g/mol、特别优选800至6000g/mol;特别是约2000g/mol的聚四氢呋喃多元醇作为载体醇。
适合制备聚合物多元醇固体部分的烯键式不饱和单体的实例有丁二烯、异戊二烯、1,4-戊二烯、1,6-己二烯、1,7-辛二烯、苯乙烯、α-甲基苯乙烯、2-甲基苯乙烯、3-甲基苯乙烯、4-甲基苯乙烯、2,4-二甲基苯乙烯、乙基苯乙烯、异丙基苯乙烯、丁基苯乙烯、苯基苯乙烯、环己基苯乙烯、苯甲基苯乙烯及类似的衍生物;取代苯乙烯,如氰基苯乙烯、硝基苯乙烯、N,N-二甲基氨基苯乙烯、乙酰氧基苯乙烯、4-乙烯基苯甲酸甲酯、苯氧基苯乙烯、对乙烯基苯基氧化物及类似的衍生物;丙烯酸酯和被取代的丙烯酸酯,如丙烯腈、丙烯酸、甲基丙烯酸、丙烯酸甲酯、丙烯酸2-羟基乙酯、甲基丙烯酸甲酯、甲基丙烯酸环己酯、甲基丙烯酸苯甲酯、甲基丙烯酸异丙酯、甲基丙烯酸辛酯、甲基丙烯腈、α-乙氧基丙烯酸乙酯、α-乙酰氨基丙烯酸甲酯、丙烯酸丁酯、丙烯酸2-乙基己酯、丙烯酸苯酯、甲基丙烯酸苯酯、丙烯酰胺、N,N-二甲基丙烯酰胺、N,N-二苯甲基丙烯酰胺、N-丁基丙烯酰胺、甲基丙烯酰甲酰胺及类似的衍生物;乙烯基酯、乙烯基醚、乙烯基酮等,如乙酸乙烯酯、丁酸乙烯酯、乙酸异丙烯酯、甲酸乙烯酯、丙烯酸乙烯酯、甲基丙烯酸乙烯酯、甲氧基乙酸乙烯酯、苯甲酸乙烯酯、乙烯基甲苯、乙烯基萘、乙烯基甲基醚、乙烯基丙基醚、乙烯基丁基醚、乙烯基2-乙基己基醚、乙烯基苯基醚、乙烯基2-甲氧基乙基醚、甲氧基丁二烯、乙烯基2-丁氧基乙基醚、2,4-二氢-1,2-吡喃、2-丁氧基-2’-乙烯氧基二乙基醚、乙烯基甲基酮、乙烯基乙基酮、乙烯基苯基酮、乙烯基乙基砜、N-甲基-N-乙烯基乙酰胺、N-乙烯基吡咯烷酮、乙烯基咪唑、二乙烯基亚砜(dinviyl sulfoxide)、二乙烯基砜、乙烯基磺酸钠、乙烯基磺酸甲酯、N-乙烯基吡咯、膦酸乙烯酯及类似的衍生物;富马酸二甲酯、马来酸二甲酯、马来酸、巴豆酸、富马酸、衣康酸、衣康酸单甲酯、甲基丙烯酸叔丁基氨基乙酯、甲基丙烯酸二甲基氨基乙酯、丙烯酸缩水甘油酯、烯丙醇、衣康酸的乙二醇单酯、乙烯基吡啶及类似的衍生物。优选的烯键式不饱和单体有苯乙烯、丙烯腈、丙烯酸酯和丙烯酰胺,特别是比例为1:3至3:1的苯乙烯和丙烯腈。还优选向聚合反应中添加大分子单体。如果合适,所述聚合反应还使用一种缓和剂和一种自由基引发剂进行。
如果伴随使用聚合物多元醇,基于组分b1)计,则其伴随用量一般最高达80重量%、优选5至20重量%。
制备聚氨酯泡沫中还可存在发泡剂d)。如果合适,所述发泡剂包括水。使用的发泡剂d)不仅可包括水,而且还可另外包括熟知的化学和/或物理发泡剂。化学发泡剂是通过与异氰酸酯进行反应而形成气态产物的化合物,例如水或甲酸。物理发泡剂是已在制备聚氨酯的起始物质中溶解或乳化、并在形成聚氨酯的条件下蒸发的化合物。它们为例如烃、卤代烃和其他化合物,如全氟化烷烃(如全氟己烷)、氯氟烃,以及醚、酯、酮和/或缩醛,例如具有4至8个碳原子的脂(环)族烃,或氟代烃,例如产自Solvay Fluorides LLC的365mfc。在一个优选实施方案中,使用的发泡剂包括含有至少一种所述发泡剂和水的混合物,特别是仅使用水作为发泡剂。如果不使用水作发泡剂,则优选仅使用物理发泡剂。
在一个优选实施方案中,水的含量为0.025至3重量%、优选0.05至2重量%、特别优选0.1至1.5重量%、特别是0.15至1重量%,基于组分a)至f)的总重量计。
优选用于制备所述聚氨酯泡沫的催化剂e)为能够显著加速包含羟基的组分b)化合物和——如果合适——组分d)化合物与多异氰酸酯a)的反应的化合物。可提及例如以下物质:脒,如2,3-二甲基-3,4,5,6-四氢嘧啶;叔胺,如三乙胺、三丁胺、二甲基苯甲胺、N-甲基吗啉、N-乙基吗啉和N-环己基吗啉、N,N,N’,N’-四甲基乙二胺、N,N,N’,N’-四甲基丁二胺、N,N,N’,N’-四甲基己二胺、五甲基二亚乙基三胺、四甲基二氨基乙基醚、二(二甲基氨基丙基)脲、二甲基哌嗪、1,2-二甲基咪唑、1-氮杂二环[3.3.0]辛烷和优选的1,4-二氮杂二环[2.2.2]辛烷;以及链烷醇胺化合物,如三乙醇胺、三异丙醇胺、N-甲基二乙醇胺和N-乙基二乙醇胺及二甲基乙醇胺。还可使用以下物质:有机金属化合物,优选有机锡化合物,例如有机羧酸的锡(II)盐,如乙酸锡(II)、辛酸锡(II)、乙基己酸锡(II)和月桂酸锡(II);及有机羧酸的二烷基锡(IV)盐,例如二乙酸二丁基锡、二月桂酸二丁基锡、马来酸二丁基锡和二乙酸二辛基锡;以及羧酸铋,例如新癸酸铋(III)、2-乙基己酸铋和辛酸铋;或其混合物。还可使用基于钛和基于锌的催化剂,如二异丙氧基双(乙基乙酰乙酸)钛(IV)、二异丙氧基双(乙酰丙酮)钛(IV)、三异丙氧基乙酰丙酮钛(IV)、乙氧基双(乙酰丙酮)(异丙氧基)钛(ethoxybis(pentane-2,4-dionato-O,O’)(propan-2-olato)titanium)、乙酰丙酮氧化钛(IV)、丁氧基异丙氧基双(二乙酰丙酮)钛(IV)、乙氧基二异丙氧基双(二乙酰丙酮)钛(IV);以及锌的饱和或不饱和的、脂族或脂环族和芳香族羧酸盐,如环烷酸锌(II)、癸酸锌(II)、丁酸锌(II),如4-环己基丁酸锌(II)、新癸酸锌(II)、异丁酸锌(II)、苯甲酸锌(II)以及二-2,2,6,6-四甲基-3,5-庚二酸锌(II)和对甲苯磺酸锌(II)。特别优选使用辛酸锌(II)和2-乙基己酸锌(II)。此处优选彼此结合使用基于钛和基于锌的催化剂。此类结合物描述于例如EP1736489中。所述有机金属化合物可以单独地使用或优选与强碱性胺结合使用。如果组分b1)包含一种酯,则优选仅使用胺催化剂。
基于所述组分b)的重量计,优选使用0.001至5重量%、特别是0.05至2重量%的催化剂或催化剂结合物。
如果合适,助剂和/或添加剂f)也可加入制备聚氨酯泡沫的反应混合物中。可以以实例方式提及的有表面活性剂、稳泡剂、泡孔调节剂、脱模剂、填充剂、染料、颜料、水解稳定剂、气味吸收物质、香料和抑制真菌和/或抑制细菌物质。
可使用的表面活性剂的实例有用于促进起始物质均质化、并且如果合适还适用于调节泡孔结构的化合物。可以以实例方式提及的有乳化剂,例如蓖麻油硫酸酯的钠盐或脂肪酸的钠盐,及脂肪酸与胺的盐,例如二乙胺油酸盐、二乙醇胺硬脂酸盐以及二乙醇胺蓖麻油酸盐,磺酸的盐,例如十二烷基苯磺酸或二萘基甲烷二磺酸的碱金属或铵盐,以及蓖麻油酸;稳泡剂,例如硅氧烷-氧化烯共聚物和其他有机聚硅氧烷、乙氧基化烷基苯酚、乙氧基化脂肪醇、液体石蜡、蓖麻油酯或蓖麻油酸酯、土耳其红油和花生油;以及泡孔调节剂,例如石蜡、脂肪醇和二甲基聚硅氧烷。此外,含聚氧化烯和氟代烷基侧基的低聚丙烯酸酯适用于改善乳化效果和泡孔结构和/或稳定泡沫。所述表面活性剂的使用量通常为0.01至5重量份,基于100重量份的组分b)计。
可提及的发泡剂的实例有:脂肪酸酯与多异氰酸酯的反应产物、衍生自脂肪酸和含有氨基的聚硅氧烷的盐、衍生自具有至少8个碳原子的饱和或不饱和脂(环)族羧酸和叔胺的盐、以及特别是内脱模剂如羧酸酯和/或羧酰胺,所述内脱模剂通过使一种由褐煤酸和至少一种具有至少10个碳原子的脂族羧酸构成的混合物与摩尔质量为60至400g/mol的至少双官能的烷醇胺、多元醇和/或多胺发生酯化或酰胺化而制备,如EP0153639中所公开;通过由有机胺、硬脂酸的金属盐以及有机单羧酸和/或有机二羧酸或其酸酐构成的混合物的酯化或酰胺化而制备,如DE-A3607447中所公开;或通过由亚氨基化合物、羧酸的金属盐以及——如果合适——羧酸构成的混合物的酯化或酰胺化而制备,如US4,764,537所公开。
可添加的填充剂特别是颗粒大小大于50μm的增强填充剂。它们为本身已知的常规有机和无机填充剂、增强剂、加重剂、涂布剂等。可提及以下各实例:无机填充剂,例如硅酸盐矿物,例如层状硅酸盐如叶蛇纹石、膨润土、蛇纹石、角闪石、闪石、纤维蛇纹石、碳酸钙和滑石;金属氧化物如高岭土、氧化铝、氧化钛、氧化锌和氧化铁;金属盐如白垩和重晶石,以及无机颜料如硫化镉和硫化锌,以及玻璃等。优选使用高岭土(瓷土)、硅酸铝及由硫酸钡和硅酸铝构成的共沉淀物,以及天然和合成的纤维材料如硅灰石、金属丝、和特别是各种长度的玻璃纤维,上述材料如果合适还可被筛分。可使用的有机填充剂的实例有:炭黑、三聚氰胺、松脂、环戊二烯树脂和接枝聚合物,以及纤维素纤维、聚酰胺纤维、聚丙烯腈纤维、聚氨酯纤维和基于芳香族和/或脂族二羧酸酯的聚酯纤维、以及特别是碳纤维。
所述无机和有机填充剂可单独使用或以混合物的形式使用,并有利地,基于组分a)至c)的重量计,以0.5至50重量%、优选1至30重量%的量添加至反应混合物中。
此处,本发明聚氨酯通过将组分a)至f)混合并使反应混合物完成反应而制备。为制备本发明的泡沫聚氨酯,将这些材料一起以如下量混合,所述量能够使多异氰酸酯a)的NCO基团的当量数与组分b)、c)和d)的反应活性氢原子的总和的比值为1:0.8至1:1.25、优选1:0.9至1:1.15。
本发明的泡沫聚氨酯优选通过一步法借助低压或高压技术制备。为制备本发明的整皮泡沫,将起始组分a)至f)优选在15至90℃、特别优选25至55℃的温度混合,并将所述反应混合物——如果合适在升高的压力下——引入密闭模具中。所述混合可使用搅拌器或混合螺杆、或者在高压下使用所谓的逆流注射法机械地进行。模具温度有利地为20至160℃,优选30至120℃,特别优选30至60℃。
存在多种制作网球的方法。一种合适的制作方法是将反应混合物倒入金属模具中,使其增长(rise)并完成反应。在一个优选实施方案中,可使该模具沿其自身轴随机旋转或以受控方式在所有方向旋转,以实现中心对称的各向同性密度。如果合适,一种方法是使模具足够快地旋转,以使所述材料覆盖模具壁并由此向内部增长,进而使密度向球芯明显降低。脱模后,可通过多种粘合方法例如使用热熔粘合剂或使用常规丙烯酸酯体系来施用纺织布。另一种优选途径是将纺织布放入模具,将反应混合物倒入模具中,并接着进行上述过程。
加入模具中的反应混合物的量确定为使形成的整皮泡沫模制品根据DIN EN ISO845的密度为250至500g/L、优选300至470g/L、特别是320至430g/L。制备具有密实周边区域和多孔中心的模制品的密实度为1.1至8.5、优选1.3至7.0、特别是1.6至5.0。
以下实施例提供对本发明的进一步说明。
实施例
起始材料
多元醇1:聚氧化丁烯醚醇(OH值为56mg KOH/mg)
多元醇2:丙二醇起始的主要含有伯OH基团的聚醚多元醇(OH值为29mg KOH/mg)(组成:80%环氧丙烷、20%环氧乙烷)
增链剂1:单乙二醇
增链剂2:1,4-丁二醇
催化剂1:三亚乙基二胺
催化剂2:二月桂酸二甲基锡
发泡剂:水
异氰酸酯1:预聚物(54重量份4,4’-二异氰酸酯基二苯基甲烷(直链MDI)、6重量份经脲酮亚胺改性的直链MDI、40重量份线性聚氧化丁烯醚醇(OH值为56mg KOH/mg))
使用的多元醇组分由62.83重量份多元醇1、30重量份多元醇2、4.8重量份增链剂1、1重量份增链剂2、0.64重量份发泡剂、0.4重量份催化剂1、0.03重量份催化剂2、0.3重量份稳泡剂构成。
反应混合物1:
将100重量份的多元醇组分(45℃)和77重量份异氰酸酯1(40℃)相互混合,将该混合物装入毛毡衬里的金属模具(球形模具,直径6.7cm)中,从而制备网球。
储存24小时后根据DIN ISO53512测定制备样品的回弹性并列于表1中。
表1
反应混合物1 | 网球(参照) | |
球重量(g) | 57.4g | 57.9g |
回弹性(%) | 56% | 56% |
在容许公差内,由反应混合物1制备的样品不仅具有需要的重量和回弹性,而且(如图所示)还具有针对压缩变形(作用力=80N)以cm测量的ITF规格要求的耐压强度数值。当对所述聚氨酯球施加“向前”负载时,其相对于橡胶参照球的偏差仅为7%(距最佳值的最大偏差=13.7%),当对其施加“向后”负载时,偏差为8.3%(距最佳值的最大偏差=14.9%)。因此,如这些数据所示,可使用本发明的聚氨酯组合物制备网球,所述网球在比赛中的性能与常规网球相当,这也已通过现场试验得到证实。
Claims (4)
1.一种泡沫聚氨酯用于制备网球的用途,所述泡沫聚氨酯通过将以下组分混合得到一种反应混合物,并使所述反应混合物完成反应而获得:
a)有机多异氰酸酯,
b)多羟基化合物,包含
b1)聚醚多元醇,其平均OH官能度≤2.5、摩尔质量为450至12000g/mol且具有大于50%比例的伯羟基,其中所述聚醚多元醇b1)为一种由以下组分构成的混合物
b11)50至90重量%的聚四氢呋喃多元醇,和
b12)10至50重量%的聚氧丙烯-聚氧乙烯多元醇,和
b2)低分子量二元醇,其摩尔质量为52至400g/mol,和
b3)如果合适,低分子量交联剂,其含有至少3个对异氰酸酯基团有反应活性的基团,其中组分b3)在组分b)中的含量为0至5重量%,
其中组分b2)在组分b)中的含量为4至20重量%,
c)如果合适,聚合物多元醇,
d)发泡剂,
e)催化剂,和如果合适,
f)助剂和添加剂。
2.权利要求1的用途,其中所述低分子量二元醇b2)选自乙二醇、二甘醇、1,2-丙二醇或1,3-丙二醇、双丙甘醇、三丙二醇、1,4-丁二醇、1,5-戊二醇、1,6-己二醇和1,10-癸二醇。
3.权利要求1或2的用途,其中所述低分子量二元醇b2)在组分b)中的比例为5至20重量%。
4.一种网球,其包含权利要求1或2所定义的泡沫聚氨酯。
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PCT/EP2009/059755 WO2010012736A1 (de) | 2008-07-30 | 2009-07-28 | Verfahren zur herstellung polyurethanbasierter tennisbälle |
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