CN110461888A - 聚合物水分散体在高分子多孔材料界面粘结的用途 - Google Patents
聚合物水分散体在高分子多孔材料界面粘结的用途 Download PDFInfo
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- CN110461888A CN110461888A CN201780084599.3A CN201780084599A CN110461888A CN 110461888 A CN110461888 A CN 110461888A CN 201780084599 A CN201780084599 A CN 201780084599A CN 110461888 A CN110461888 A CN 110461888A
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- vinyl
- polymer dispersion
- aqueous polymer
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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Abstract
本发明涉及聚合物水分散体用于高分子多孔材料界面粘合的用途。
Description
技术领域
本发明涉及一种聚合物水分散体在高分子多孔材料界面粘结的用途。
背景技术
US6624243B2专利公开了一种由可聚合的硅烷、乙烯基酯、环氧化合物及1,3二羰基化合物单体所聚合的聚合物水分散体。该水分散体可改善墙面漆的耐刮擦性能。
US6863985B2公开了一种由可聚合的硅烷、硅油、乙烯基酯及环氧化合物聚合而成的聚合物水分散体。该分散体具有较强的防水性、水蒸气透过性,特别适用于制备外墙漆。
WO2014071550A1描述了一种用于纺织品层状贴合的聚合物水分散体。所描述的聚合物由乙酸乙烯酯和乙烯的聚合单体及聚氨酯聚合而成。根据该专利披露的湿剥离强度检测方法,所述聚合物水分散体粘结的产品,160℃、6秒贴合,经过180℃条件下热处理2分钟,随后冷水浸泡半小时,得到产品的湿剥离强度在6-8N之间。
CN102869828B公开了一种地毯涂料组合物,其中包含乙酸乙烯酯、乙烯和不饱和硅烷共聚单体的乳液聚合得到的互聚物,其中不饱和硅烷共聚单体能够有效地改变互聚物的分子量、支化和/或流动性能使得互聚物形成的膜在110℃时呈现出小于125%的伸长值。
发明内容
一种聚合物水分散体在提高高分子多孔材料界面粘结耐水性能的用途,所述聚合物由包含a-d组分的组合物聚合而成:
a.一种或几种单体,选自C1-C15含直链或侧链的乙烯基烷基羧酸酯、乙烯芳族化合物、烯烃、二烯烃、卤代乙烯化合物组成的组;
b.可聚合的可水解的含硅化合物,选自含不饱和乙烯基可水解的有机硅化合物;
c.可聚合的阴离子乳化剂;
可选的d.乙烯基的环氧化合物;
其中高分子多孔材料界面粘结是纤维纺织材料和高分子发泡材料中一种或多种相同或不同材料界面之间的粘结;优选人造纤维纺织材料、人造纤维无纺布材料、天然纤维纺织材料、天然纤维无纺布材料、再生纤维素材料、EVA乙烯醋酸乙烯共聚物海绵、PU聚氨酯海绵中一种或多种相同或不同材料界面之间的粘结。
如上所述用途,其中提高耐水性能是指满足如下条件:按照ST-4和ST-3的测试条件得到的湿剥离强度与干剥离强度的比值为湿剥离保留,湿剥离保留大于等于0.5。
如上所述用途,其中提高耐水性能是指,按照ST-4测试条件,湿剥离强度大于等于30N/inch。
高分子多孔材料界面粘结得到复合材料产品。一些复合材料产品在使用环境中需要经常与水接触,或者经常需要清洗。这些复合材料的应用领域包括例如鞋衬里、鞋垫、运动型服装等。耐水性差的复合材料产品遇水容易发生脱胶,即材料界面分离。产品的使用寿命低。
如上所述用途,高分子多孔材料界面粘结优选为纤维纺织材料与高分子发泡材料的层状粘结贴合。
如上所述用途,高分子多孔材料界面粘结优选为聚酯或腈纶或棉布纺织材料,与平坦的EVA乙烯-醋酸乙烯共聚物海绵界面之间的粘结。
如上所述用途,其中将聚合物水分散体施于高分子多孔材料界面之间,得到的产品与热源接触加热一段时间。
如上所述用途,其中不包括地毯领域。大多数常规地毯包含具有切割或未切割毛圈形式的纱线簇绒的主底衬,这些纱绒从该底衬向上延伸形成绒毛表面。在制造簇绒地毯时,通过簇绒针将纱线***主底衬中并向该主底衬施涂预涂层或粘结剂。在制造非簇绒或粘结的绒毛地毯的情况下,将纤维嵌入并实际上通过粘结剂组合物将该纤维固定。
如上所述用途,高分子多孔材料界面粘结领域不包括高分子多孔材料的本体粘结领域。高分子多孔材料的本体粘结主要指直径小于5毫米的纤维状高分子材料的粘结。例如制造无纺布过程中用粘结剂将木浆纤维、人造丝、棉、羊毛、乙酸酯纤维等粘结成型得到无纺布;或者造纸过程中用粘结剂将纸浆纤维粘结成型得到纸网、纸张或者纸板。
如上所述用途,其中将聚合物水分散体施于高分子多孔材料界面之间,得到的产品在150-200℃之间与热源接触加热处理25秒至120秒之间,完成干燥步骤;或者将将聚合物水分散体施于高分子多孔材料界面之间,得到的产品在100-110℃之间与热源接触加热处理20分钟-30分钟之间,完成干燥步骤。
如上所述用途,其中采用辊式涂布机将聚合物水分散体施于高分子多孔材料界面之间施加一定压力,并完成干燥步骤。
如上所述用途,采用辊式涂布机完成干燥步骤之后,无需进一步热压处理。
如上所述用途,其中聚合物水分散体的涂布量在120-210g/m2之间。
如上所述用途,其中根据ST-1测试方法,该聚合物水分散体干燥物的玻璃转化温度Tg在-2-4℃之间。使用这种聚合物水分散体粘结纤维纺织材料和高分子发泡材料之间的界面,粘结后得到的产品手感柔软。
如上所述用途,其中聚合物水分散体是乳液,稳定性良好,在50℃14天储存条件下,布氏粘度变化率小于30wt%。布氏粘度变化率指:50℃储存条件下,第1天布氏粘度与第14天布氏粘度的差值,除以第1天布氏粘度。
如上所述用途,其中根据ST-2布式粘度测试方法,聚合物水分散体的布式粘度在1500-10,000mPa.s之间。
聚合物水分散体的粘度太低时,生产过程中涂布辊的取胶量小,产品粘结效果不好。聚合物水分散体的粘度太高时,涂布辊的取胶量大,产品的涂布量过多,聚合物水分散体的耗用成本高,不经济。
如上所述用途,其中组分a.一种或几种单体,选自包含乙烯基酯、乙烯、氯乙烯、丙烯酸酯的组;更优选组分a.两种单体选自乙酸乙烯酯、乙烯。
如上所述用途,其中组分c.可聚合的阴离子乳化剂是含不饱和基团的烷基磺酸盐;优选乙烯基磺酸钠、1-烯丙氧基-2-羟丙基磺酸盐、2-丙烯酰胺-2-甲基丙磺酸钠;特别优选乙烯基磺酸钠。
如上所述用途,其中组分b.可聚合的可水解的含硅化合物和组分c.可聚合的阴离子乳化剂的干物质重量比的范围在1-2之间。
如上所述用途,其中组分b.可聚合的可水解的含硅化合物和组分d.乙烯基的环氧化物的干物质重量比在0.5-0.7之间。
如上所述用途制备得到的复合材料,其中按照ST-4和ST-3的测试条件得到的湿剥离强度与干剥离强度的比值为湿剥离保留,湿剥离保留大于等于0.5。
如上所述用途制备得到的复合材料,其中根据ST-4测试方法得到湿剥离强度大于等于30N/inch,且湿剥离保留大于等于0.5。使用这种聚合物水分散体粘结纤维纺织材料和高分子发泡材料之间的界面,粘结后得到的产品具有良好的耐水性。
本发明所述的用于高分子多孔材料界面粘结的聚合物水分散体,其中聚合物由包含a-d组分的组合物聚合而成。
a.一种或几种单体,选自C1-C15含直链或侧链的乙烯基烷基羧酸酯,乙烯芳族化合物,烯烃,二烯烃,卤代乙烯化合物组成的组;
优选的C1-C15含直链或侧链的乙烯基烷基羧酸酯选自乙酸乙烯酯,丙酸乙烯酯,丁酸乙烯酯,2-乙基己酸乙烯酯,月桂酸乙烯酯,乙酸1-甲基乙烯酯,新戊酸乙烯酯和最多具有10个碳原子的α-支链单羧酸乙烯酯,例如VeoVa9或VeoVa10组成的组,特别优选乙酸乙烯酯。
适当的共聚单体甲基丙烯酸酯或丙烯酸酯是具有1至15个碳原子、非支化或支化醇的酯,例如丙烯酸甲酯、甲基丙烯酸甲酯、丙烯酸乙酯、甲基丙烯酸乙酯、丙烯酸丙酯、甲基丙烯酸丙酯、丙烯酸正丁酯、甲基丙烯酸正丁酯、丙烯酸2-乙基己酯和丙烯酸降冰片酯。其中优选丙烯酸甲酯、甲基丙烯酸甲酯、丙烯酸正丁酯和丙烯酸2-乙基己酯。
所述的组分a.也可以聚合形成乙酸乙烯基酯与乙烯的共聚物、乙酸乙烯基酯与乙烯和一种或多种其它乙烯基单体的共聚物,例如乙酸乙烯基酯-乙烯-丙烯酸酯共聚物、乙酸乙烯基酯-乙烯-氯乙烯的共聚物共聚物。
优选的组分b.可聚合的可水解的含硅化合物选自含不饱和乙烯基可水解的有机硅化合物;更优选自一种或几种由乙烯基三甲氧基硅烷、乙烯基二甲氧基甲基硅烷、乙烯基甲氧基二甲基硅烷、乙烯基三乙氧基硅烷、乙烯基二乙氧基甲基硅烷、乙烯基乙氧基二甲基硅烷、乙烯基三(甲基乙氧基)硅烷、乙烯基三(甲基异丙氧基)硅烷、3-甲基丙烯酰氧基丙基三甲氧基硅烷、3-甲基丙烯酰氧基丙基三乙氧基硅烷组成的组。
最优选的组分b是乙烯基三甲氧基和/或乙烯基三乙氧基硅烷。
组分c.可聚合的阴离子乳化剂选自含不饱和基团的烷基磺酸盐;优选乙烯基磺酸钠、1-烯丙氧基-2-羟丙基磺酸盐、2-丙烯酰胺-2-甲基丙磺酸钠;特别优选乙烯基磺酸钠。
可选的组分d.乙烯基的环氧化合物选自丙烯酸缩水甘油酯、甲基丙烯酸缩水甘油酯、烯丙基缩水甘油醚、乙烯基缩水甘油醚、氧化乙烯基环己烯、氧化月桂烯。
所述聚合物通过溶液、乳液或悬浮聚合方法制备,优选通过乳液聚合方法制备,聚合温度通常为20℃至100℃,优选为45℃至80℃。气相聚合单体如乙烯、1,3-丁二烯或氯乙烯的聚合也可以在通常为5bar至100bar的绝压下进行。聚合所需之pH值一般在2.5-10之间,优选为3-8,这可以以已知的方法通过酸、碱或常规的缓冲盐例如碱金属磷酸盐或碱金属碳酸盐来确定。
聚合反应通过乳液聚合或悬浮聚合中常规的水溶性或可溶于单体的引发剂或氧化还原引发剂的组合来引发。水溶性引发剂的实例为过硫酸的钠、钾和铵盐、过氧化氢、叔丁基过氧化物、叔丁基过氧化氢、过二磷酸钾、过氧化新戊酸叔丁基酯、偶氮二异丁腈。在每种情况下所述引发剂的用量通常为单体总干重的0.01至3wt%。
作为氧化还原引发剂,使用前述引发剂与还原剂的组合。适合的还原剂为碱金属或铵的亚硫酸盐、碱金属或铵的亚硫酸氢盐、碱金属或铵的次硫酸的衍生物、或碱金属或铵的亚磺酸盐。在每种情况下所述还原剂的用量通常为组分a.单体总干重的0.01至3wt%。
为了控制分子量可以在聚合过程中使用调节物质。如果使用调节物质,其用量通常为组分a.单体总干重的0.01至5.0wt%,并且是单独引入或与反应成分预混合。所述物质的实例为正十二烷基硫醇、叔十二烷基硫醇、巯基丙酸、巯基丙酸甲酯、异丙醇和乙醛。
适合用于聚合的保护胶体为聚乙烯醇、聚乙烯醇缩乙醛、聚乙烯基吡咯烷酮、水溶性形式的多糖例如淀粉(直链淀粉和支链淀粉)、纤维素及其羧甲基、甲基、羟乙基、羟丙基衍生物、糊精和环糊精。
聚合反应可分批或连续进行聚合。
聚合结束之后,可以用公知的方法进行后聚合以除去残余单体,通常通过由氧化还原催化剂引发的后聚合方法进行。也可以用蒸馏的方法除去挥发性残余单体,蒸馏优选在减压条件下进行,并且如果合适的话,使用通过聚合混合物的惰性夹带气体例如空气、氮气或蒸汽。以这种方式获得的聚合物水分散体的固含量为40至70wt%。
可以在本发明的聚合物水分散体添加保护胶体(作为喷洒助剂)、消泡剂、抗结块剂,随后制备水中可再分散的聚合物粉末。该工艺是常规的流化床干燥、冻干或喷干工艺。
制样和测试方法
玻璃转化温度制样和测试方法ST-1:
取一定量聚合物水分散体样品,25℃干燥过夜,然后在真空烘箱40℃静置24小时得到聚合物水分散体干燥物。
取8-15mg聚合物水分散体干燥物,根据ISO11357-1 2014,在氮气保护条件下,用NETZSCH F203,封闭型样品池,在10K/min加热速率下从-80℃升温至100℃,得到聚合物水分散体干燥物的玻璃转化温度Tg。
检测方法ST-2布式粘度:
根据GB/T 11175-2002,利用Brookfield RV/DV旋转粘度计,在25℃、20转/分钟条件下,使用4号转子测试样品的粘度。
实验室剥离强度制样方法:
参照ISO11339-2010改良的测试方法,将一块纯棉白布织物剪裁成20cm*35cm的片状。将纯棉白布平铺在玻璃板上,上下两端用1.8cm宽的3M电工胶带固定。用刮墨刀将聚合物水分散体涂抹在白布上方,用40um的刮棒刮平,计时1分钟后,再涂抹一层聚合物水分散体在白布上方,用50um刮棒刮平。计时1min后,将白布对折,用2kg的压辊水平压两次。放入烘箱中,在105℃条件热处理30mins后,取出布样,裁剪成2.54cm*35cm的干布样。
测试方法ST-3干剥离强度:
参考ISO11339-2010图1所示方法采用上述干布样,在山东兰光测试XLW(G)-PC型智能电子拉力机上测180°的剥离强度。干布样垂直拉伸距离为40mm、宽度25.4mm(即1inch),前后各多2mm不取值。拉伸速度为100mm/min。
测试方法ST-4湿剥离强度:
制备湿布样:将上述干布样放置在25℃的水中浸泡1小时后取出得到。
参考ISO11339-2010图1所示方法采用湿布样在山东兰光测试XLW(G)-PC型智能电子拉力机上测180°剥离后得到湿剥离强度。
工业制样方法:使用工业辊式涂布机
滚筒长度:L=6.28m
热处理温度:T=160℃
热处理时间:15~30s
涂布量:120g/m2
使用瓦克化学公司市售产品EP706K(该产品不属于本发明权利要求书所描述的聚合物水分散体)作为粘结剂,筛选与工业制样方法最接近的实验室剥离强度制样方法。由表1测试数据可知,105℃条件热处理30mins的实验室剥离强度制样方法基本等效于工业制样方法。
表1
实施例
实施例1-9和对比例C1-C3中的聚合物水分散体按照表2中的基本配方配置而成。表2基本配方中含有单体种类、各单体用量、保护胶体种类、引发***、各原料初始进料用量、后续进料用量等。
本发明所述用量若无特别说明,均以重量份计算。
在表2和3中,若无特别说明,则按以乙酸乙烯酯单体重量为100份作为参比,计算各原料的重量份。
在表2和3中,溶液浓度为溶质和溶液的重量百分比。
Mersolat H95,主要是仲烷基磺酸钠化合物的混合物,其中仲烷基磺酸钠化合物中饱和烷基的平均链长为15个碳原子,由Rhein Chemie提供;
XL 10,乙烯基三甲氧基硅烷,由瓦克化学公司提供;
GMA,甲基丙烯酸缩水甘油酯,由国药试剂公司提供;
Genapol 3214,烷基醇聚氧乙烯醚,烷基链长约为C13(Tridecyl alcoholethoxylate)HLB值约为17,由Clariant公司提供;
RHODASURF 6530,烷基醇聚氧乙烯醚(Aliphatic alcohol ethoxylates),HLB值约为17,由Rhodia Solvay Group公司提供;
聚乙烯醇25/88,88wt%醇解度聚乙烯醇,其4wt%水溶液在20℃时根据DIN 53015测得的粘度为25mPa·s,使用前配成10.3wt%的水溶液。
Foamaster 223,矿物油消泡剂,由BASF公司提供。
EP 706K是乙烯-乙酸乙烯酯聚合物水分散体,由瓦克化学公司提供。
表2基本配方
*表2中的乙烯用量,指各例中乙烯气体投料量。
实施例1-9和对比例C1-C3主要调整的原料参见表3,实施步骤类似实施例1。
表3
实施例1
在5升反应釜中加入584.43g去离子水,443g 10.3wt%聚乙烯醇25/88,13gMersolate H95,110.77g 65wt%Genopol 3214,20.1g 25wt%乙烯基磺酸钠,2.78g 2wt%乙二胺四乙酸钠,20.3g醋酸钠的提前料。将提前料混合均匀并用醋酸将pH调至5。
将反应釜加热到70℃,加入252g乙酸乙烯酯和400g乙烯气体,并保持反应釜压力在45Bar以下。
升温至70℃,同时用泵滴加1.25wt%过硫酸铵水溶液和5wt%2-羟基-2-亚磺酸乙酸二钠盐水溶液后引发反应并持续滴加直至反应结束。引发反应以12.6g/分钟的速率加入2265.6g乙酸乙烯酯,以2.5g/分钟的速率加入318.76g去离子水,115g 10.3wt%聚乙烯醇25/88,7.12g GENIOSIL XL 10和12.2g甲基丙烯酸缩水甘油酯组成的混合溶液。
反应4小时后,转入脱气罐,加入1g消泡剂Foamaster 223,脱气30分钟后出料得到聚合物水分散体。
得到的聚合物水分散体,在室温条件储存14天后,测试pH值在4.5-5之间。
表4是实施例1-9和对比例C1-C3的性能测试结果
表4
按照对比例C3制备得到的产品在室温条件储存1天后,就出现分层破乳,无法用于实际生产。
Claims (12)
1.一种聚合物水分散体在提高高分子多孔材料界面粘结耐水性能的用途,所述聚合物由包含a-d组分的组合物聚合而成:
a.一种或几种单体,选自C1-C15含直链或侧链的乙烯基烷基羧酸酯、乙烯芳族化合物、烯烃、二烯烃、卤代乙烯化合物组成的组;
b.可聚合的可水解的含硅化合物,选自含不饱和乙烯基可水解的有机硅化合物;
c.可聚合的阴离子乳化剂;
可选的d.乙烯基的环氧化合物;
其中高分子多孔材料界面粘结是纤维纺织材料和高分子发泡材料中一种或几种相同或不同材料界面之间的粘结;优选人造纤维纺织材料、人造纤维无纺布材料、天然纤维纺织材料、天然纤维无纺布材料、再生纤维素材料、乙烯醋酸乙烯(EVA)共聚物海绵和聚氨酯海绵中一种或多种相同或不同材料界面之间的粘结。
2.如权利要求1所述用途,其中提高耐水性能是指满足如下条件:按照ST-4和ST-3的测试条件得到的湿剥离强度与干剥离强度的比值为湿剥离保留,湿剥离保留大于等于0.5。
3.如权利要求1或2所述用途,其中将聚合物水分散体施于高分子多孔材料界面之间,得到的产品在150-200℃之间与热源接触加热处理25秒至120秒之间,完成干燥步骤;或者将将聚合物水分散体施于高分子多孔材料界面之间,得到的产品在100-110℃之间与热源接触加热处理20分钟-30分钟之间,完成干燥步骤。
4.如权利要求1或2所述用途,其中采用辊式涂布机将聚合物水分散体在压力下施于高分子多孔材料界面之间,并完成干燥步骤。
5.如权利要求1或2或4所述用途,其中根据ST-1测试方法,该聚合物水分散体干燥物的玻璃转化温度Tg在-2-4℃之间。
6.如权利要求1或2或4所述用途,根据ST-2布式粘度测试方法,聚合物水分散体的布式粘度在1500-10,000mPa.s之间;在50℃ 14天储存条件下,布氏粘度变化率小于30wt%。
7.如权利要求1或2或4所述用途,其中组分a.一种或几种单体,选自包含乙烯基酯、乙烯、氯乙烯、丙烯酸酯的组;更优选组分a.是乙酸乙烯酯和乙烯。
8.如权利要求1或2或4所述用途,其中组分c.可聚合的阴离子乳化剂选自含不饱和基团的烷基磺酸盐;优选乙烯基磺酸钠、1-烯丙氧基-2-羟丙基磺酸盐、2-丙烯酰胺-2-甲基丙磺酸钠;特别优选乙烯基磺酸钠。
9.如权利要求1或2或4所述用途,其中组分b.可聚合的可水解的含硅化合物和组分c.可聚合的阴离子乳化剂的干物质重量比的范围在1-2之间。
10.如权利要求9所述用途,其中组分b.可聚合的可水解的含硅化合物和组分d.乙烯基的环氧化物的干物质重量比在0.5-0.7之间。
11.如权利要求1-10任一所述用途制备得到的复合材料,其中按照ST-4和ST-3的测试条件得到的湿剥离强度与干剥离强度的比值为湿剥离保留,湿剥离保留大于等于0.5。
12.如权利要求11所述用途制备得到的复合材料,其中根据ST-4测试方法得到湿剥离强度大于等于30N/inch,且湿剥离保留大于等于0.5。
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