CN113166437A - 吸水性树脂颗粒 - Google Patents
吸水性树脂颗粒 Download PDFInfo
- Publication number
- CN113166437A CN113166437A CN201980081688.1A CN201980081688A CN113166437A CN 113166437 A CN113166437 A CN 113166437A CN 201980081688 A CN201980081688 A CN 201980081688A CN 113166437 A CN113166437 A CN 113166437A
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- water
- mass
- resin particles
- absorbent resin
- polymerization
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Abstract
本发明公开了一种吸水性树脂颗粒,其包含具有源自烯属不饱和单体的结构单元的交联聚合物,所述烯属不饱和单体包含选自由(甲基)丙烯酸及其盐组成的组中的至少一种化合物,其中,相对于所述交联聚合物中的单体单元总量,(甲基)丙烯酸及其盐的比例为70~100摩尔%,在减压下水分保持试验中,保水率6小时值为55质量%以上,生理盐水保水量为32~70g/g。
Description
技术领域
本发明涉及一种吸水性树脂颗粒。
背景技术
吸水性树脂用于纸尿布等卫生用品的领域。例如,专利文献1中公开了一种吸收性物品,其具有透液性表层、不透液性防漏层及保液性吸收层,在所述吸收性物品中,该吸收层由遇水不溶胀的亲水性纤维或亲水性发泡体、或者遇水溶胀后进行离心脱水时的保水量为0.7g/g以下的亲水性纤维或亲水性发泡体及高吸水性聚合物组成,使上述吸收性物品吸收生理盐水10g,并在5分钟后进行离心脱水时的该生理盐水的固定化率为90%以上。
现有技术文献
专利文献
专利文献1:日本特开2002-165837号公报
发明内容
本发明要解决的技术问题
在专利文献1中进行评价的生理盐水的固定化率为表示吸收了5分钟生理盐水的吸收性物品在离心脱水后保持了多少水的值。然而,认为该值表示通过离心脱水将构成吸收性物品的各材质未能充分固定化(保持)的水、即存在于材质表层或材质间的剩余的水去除之后的保水能力,但是尚未对吸水性树脂颗粒自身将吸收到其内部的水分再次释放到外部的内容进行任何研究。因此,在抑制吸收性物品的闷热方面存在改善的余地。
本发明的目的在于提供一种能够抑制用作卫生用品时的闷热的吸水性树脂颗粒、以及使用了该吸水性树脂颗粒的吸收体及吸收性物品。
解决技术问题的技术手段
本发明的吸水性树脂颗粒在通过下述测定方法进行的减压下水分保持试验中,保水率6小时值为55质量%以上。
向在100ml烧杯内以600rpm进行搅拌的生理盐水38g中投入吸水性树脂颗粒2g,且从旋涡消失的时刻起在25℃下静置30分钟,制作溶胀凝胶。将上述溶胀凝胶20g放入12cm×10cm的EDANA WSP241.2R3(12)中规定的无纺布制的茶包内,封袋后作为评价样品,测定质量。将放置在筛上的上述评价样品置于35℃、内压0.2kPa的真空干燥机内,并每1小时测定上述评价样品的质量。
溶胀凝胶量(g/g)=(评价样品质量(g)-皮重(g))/所测定的溶胀凝胶中包含的吸水性树脂颗粒干燥质量(g)
保水率(%)=(减压后溶胀凝胶量(g/g)/初始溶胀凝胶量(g/g))×100
上述吸水性树脂颗粒的生理盐水保水量可以为30~70g/g。
本发明还提供一种含有上述吸水性树脂颗粒的吸收体。
本发明还提供一种具备上述吸收体的吸收性物品。
上述吸收性物品可以为尿布。
发明效果
根据本发明,提供一种能够抑制用作卫生用品时的闷热的吸水性树脂颗粒、以及使用了该吸水性树脂颗粒的吸收体及吸收性物品。
附图说明
图1为表示吸收性物品的一个实例的剖面图。
具体实施方式
以下,对本发明的适宜的实施方案进行详细说明。但本发明并不限定于以下的实施方案。
在本说明书中,将“丙烯酸”及“甲基丙烯酸”统一记作“(甲基)丙烯酸”。“丙烯酸酯”及“甲基丙烯酸酯”也同样记作“(甲基)丙烯酸酯”。在本说明书中以区间记载的数值范围中,某区间的数值范围的上限值或下限值能够与其他区间的数值范围的上限值或下限值任意组合。在本说明书中所记载的数值范围中,其数值范围的上限值或下限值可以替换为实施例中所示的值。“水溶性”是指25℃下在水中显示5质量%以上的溶解性。在本说明书中例示的材料可以单独使用,也可以组合使用两种以上。关于组合物中的各成分的含量,当组合物中存在多种与各成分相对应的物质时,只要没有特别说明,则表示组合物中存在的该多种物质的合计量。
本实施方案的吸水性树脂颗粒在通过下述测定方法进行的减压下水分保持试验中,保水率6小时值为55质量%以上。更具体的测定方法在后述实施例中示出。
向在100ml烧杯内以600rpm进行搅拌的生理盐水38g中投入吸水性树脂颗粒2g,且从旋涡消失的时刻起在25℃下静置30分钟,制作溶胀凝胶。将上述溶胀凝胶20g放入12cm×10cm的EDANA WSP241.2R3(12)中规定的无纺布制的茶包内,封袋后作为评价样品,并测定质量作为初始值。将放置在筛上的上述评价样品置于35℃、内压0.2kPa的真空干燥机内,并每1小时测定上述评价样品的质量。
溶胀凝胶量(g/g)=(评价样品质量(g)-皮重(g))/所测定的溶胀凝胶中包含的吸水性树脂颗粒干燥质量(g)
保水率(%)=(减压后溶胀凝胶量(g/g)/初始溶胀凝胶量(g/g))×100
作为上述茶包,使用EDANA WSP241.2R3(12)中规定的无纺布制的包。即,为一种没有开口且能够热封的无纺布制的包,该无纺布的克重为16.5±1.5g/m2,压力损失124Pa下的透气度为230±50l/分钟/100cm2。作为这种茶包,具体而言,例如能够使用将NIPPONPAPER PAPYLIA CO.,LTD.制造的Heat Pac(MWA18:18gsm)裁剪成规定尺寸,根据需要弯折,且通过热封密封了各个边的茶包。
本实施方案的吸水性树脂即使在减压下的6小时后这样的严酷条件下也具有高保水率,可以说具有不易将一经吸收的水分释放到外部的性质。因此,用作尿布等卫生用品的构成材料时,所吸收的水分不易释放到外部,且能够减少使用时的闷热。
保水率6小时值可以为57质量%以上,优选为58质量%以上,更优选为60质量%以上。保水率6小时值例如可以为80质量%以下。
从抑制闷热的角度出发,本实施方案的吸水性树脂颗粒的生理盐水的保水量可以为30g/g以上、32g/g以上、35g/g以上、38g/g以上、39g/g以上、40g/g以上、41g/g以上、42g/g以上、44g/g以上或46g/g以上。吸水性树脂颗粒的生理盐水的保水量可以为70g/g以下、65g/g以下、60g/g以下、55g/g以下或52g/g以下。生理盐水的保水量可以为30~70g/g、30~60g/g、30~55g/g或32~55g/g。此外,生理盐水的保水量可以为35~70g/g、38~70g/g、41~70g/g、41~65g/g、41~60g/g、42~55g/g或44~55g/g。吸水性树脂颗粒的生理盐水的保水量能够通过后述的实施例中所记载的方法测定。
本实施方案的吸水性树脂颗粒的中值粒径例如可以为250~850μm、300~700μm或300~600μm。本实施方案的吸水性树脂颗粒例如可以在通过后述的制造方法获得时就具有所需的粒度分布,也可以进一步进行使用了基于筛的分级的粒度调节等操作,由此将粒度分布调节为规定的粒度分布。
本实施方案的吸水性树脂颗粒例如能够包含使含有烯属不饱和单体的单体聚合而得到的交联聚合物。即,本实施方案的吸水性树脂颗粒能够具有源自烯属不饱和单体的结构单元。
作为使上述单体聚合的方法,可列举出反相悬浮聚合法、水溶液聚合法、本体聚合法、沉淀聚合法等。其中,从确保所获得的吸水性树脂颗粒的良好的吸水特性及容易控制聚合反应的角度出发,优选反相悬浮聚合法或水溶液聚合法。以下,作为使烯属不饱和单体聚合的方法,以反相悬浮聚合法为例进行说明。
烯属不饱和单体优选为水溶性,例如可列举出(甲基)丙烯酸及其盐、2-(甲基)丙烯酰胺-2-甲基丙磺酸及其盐、(甲基)丙烯酰胺、N,N-二甲基(甲基)丙烯酰胺、(甲基)丙烯酸2-羟乙酯、N-羟甲基(甲基)丙烯酰胺、聚乙二醇单(甲基)丙烯酸酯、N,N-二乙基氨基乙基(甲基)丙烯酸酯、N,N-二乙基氨基丙基(甲基)丙烯酸酯、二乙基氨基丙基(甲基)丙烯酰胺等。烯属不饱和单体含有氨基时,该氨基可以被季铵化。上述单体所具有的羧基及氨基等官能团能够在后述的表面交联工序中作为能够交联的官能团而发挥作用。这些烯属不饱和单体可以单独使用,也可以组合使用两种以上。
上述之中,从工业上容易获得的角度出发,烯属不饱和单体优选包含选自由丙烯酸及其盐、甲基丙烯酸及其盐、丙烯酰胺、甲基丙烯酰胺以及N,N-二甲基丙烯酰胺组成的组中的至少一种化合物,更优选包含选自由丙烯酸及其盐、甲基丙烯酸及其盐以及丙烯酰胺组成的组中的至少一种化合物。从进一步提高吸水特性的角度出发,进一步优选烯属不饱和单体包含选自由丙烯酸及其盐、以及甲基丙烯酸及其盐组成的组中的至少一种化合物。
作为单体,可以使用一部分除了上述烯属不饱和单体以外的单体。这样的单体例如能够混合于包含上述烯属不饱和单体的水溶液中而使用。优选烯属不饱和单体的使用量相对于单体总量为70~100摩尔%。其中,更优选(甲基)丙烯酸及其盐相对于单体总量为70~100摩尔%。
通常,烯属不饱和单体适宜制成水溶液而使用。通常,只要将包含烯属不饱和单体的水溶液(以下,称为单体水溶液)中的烯属不饱和单体的浓度设为20质量%以上且饱和浓度以下即可,优选为25~70质量%,更优选为30~55质量%。关于所使用的水,例如可列举出自来水、蒸馏水、离子交换水等。
对于单体水溶液而言,当所使用的烯属不饱和单体包含酸基时,可以利用碱性中和剂中和该酸基而使用。从提高所获得的吸水性树脂颗粒的渗透压,并进一步提高保水量等吸水特性的角度出发,烯属不饱和单体中的基于碱性中和剂的中和度为烯属不饱和单体中的酸性基团的10~100摩尔%,优选为50~90摩尔%,更优选为60~80摩尔%。作为碱性中和剂,例如可列举出氢氧化钠、碳酸钠、碳酸氢钠、氢氧化钾、碳酸钾等碱金属盐;氨等。为简化中和操作,可以将这些碱性中和剂制成水溶液的状态来使用。上述碱性中和剂可以单独使用,也可以组合使用两种以上。例如能够通过将氢氧化钠、氢氧化钾等的水溶液滴加到上述单体水溶液中并混合,由此进行烯属不饱和单体的酸基的中和。
在反相悬浮聚合法中,在表面活性剂的存在下将单体水溶液分散于烃分散介质中,并利用自由基聚合引发剂等而进行烯属不饱和单体的聚合。作为自由基聚合引发剂,例如能够使用水溶性自由基聚合引发剂。在聚合时可以使用内部交联剂。
作为表面活性剂,例如可列举出非离子表面活性剂及阴离子表面活性剂。作为非离子表面活性剂,例如可列举出山梨糖醇酐脂肪酸酯、(聚)甘油脂肪酸酯(“(聚)”表示具有和不具有前缀“聚”的这两种情况。以下相同)、蔗糖脂肪酸酯、聚氧乙烯山梨糖醇酐脂肪酸酯、聚氧乙烯甘油脂肪酸酯、山梨醇脂肪酸酯(sorbitol fatty acid eater)、聚氧乙烯山梨醇脂肪酸酯(polyoxyethylene sorbitol fatty acid ester)、聚氧乙烯烷基醚、聚氧乙烯烷基苯基醚、聚氧乙烯蓖麻油、聚氧乙烯氢化蓖麻油、烷基烯丙基甲醛缩合聚氧乙烯醚、聚氧乙烯聚氧丙烯嵌段共聚物、聚氧乙烯聚氧丙基烷基醚及聚乙二醇脂肪酸酯等。作为阴离子表面活性剂,例如可列举出脂肪酸盐、烷基苯磺酸盐、烷基甲基牛磺酸盐、聚氧乙烯烷基苯基醚硫酸酯盐、聚氧乙烯烷基醚磺酸盐、聚氧乙烯烷基醚的磷酸酯及聚氧乙烯烷基烯丙基醚的磷酸酯等。其中,从W/O型反相悬浮的状态良好、容易以适宜的粒径获得吸水性树脂颗粒、工业上容易获得的角度出发,表面活性剂优选包含选自由山梨糖醇酐脂肪酸酯、聚甘油脂肪酸酯及蔗糖脂肪酸酯组成的组中的至少一种化合物。进一步,从提高所获得的吸水性树脂颗粒的吸水特性的角度出发,表面活性剂更优选包含蔗糖脂肪酸酯。这些表面活性剂可以单独使用,也可以组合使用两种以上。
从可充分获得与使用量相对应的效果且经济性的角度出发,相对于100质量份的烯属不饱和单体水溶液,表面活性剂的量优选为0.05~10质量份,更优选为0.08~5质量份,进一步优选为0.1~3质量份。
此外,在反相悬浮聚合中,可以与上述的表面活性剂一同使用高分子类分散剂。
作为高分子类分散剂,例如可列举出马来酸酐改性聚乙烯、马来酸酐改性聚丙烯、马来酸酐改性乙烯-丙烯共聚物、马来酸酐改性EPDM(乙烯-丙烯-二稀三元共聚物)、马来酸酐改性聚丁二烯、马来酸酐-乙烯共聚物、马来酸酐-丙烯共聚物、马来酸酐-乙烯-丙烯共聚物、马来酸酐-丁二烯共聚物、聚乙烯、聚丙烯、乙烯-丙烯共聚物、氧化型聚乙烯、氧化型聚丙烯、氧化型乙烯-丙烯共聚物、乙烯-丙烯酸共聚物、乙基纤维素、乙基羟乙基纤维素等。在这些高分子类分散剂中,尤其从单体的分散稳定性方面出发,优选使用马来酸酐改性聚乙烯、马来酸酐改性聚丙烯、马来酸酐改性乙烯-丙烯共聚物、马来酸酐-乙烯共聚物、马来酸酐-丙烯共聚物、马来酸酐-乙烯-丙烯共聚物、聚乙烯、聚丙烯、乙烯-丙烯共聚物、氧化型聚乙烯、氧化型聚丙烯、氧化型乙烯-丙烯共聚物。这些高分子类分散剂可以单独使用,也可以组合两种以上。
从可充分获得与使用量相对应的效果且经济性的角度出发,相对于100质量份的烯属不饱和单体水溶液,高分子类分散剂的量优选为0.05~10质量份,更优选为0.08~5质量份,进一步优选为0.1~3质量份。
自由基聚合引发剂优选为水溶性,例如可列举出过硫酸钾、过硫酸铵、过硫酸钠等过硫酸盐;过氧化甲乙酮、过氧化甲基异丁基酮、过氧化二叔丁基、过氧化叔丁基异丙苯、过氧化乙酸叔丁酯、过氧化异丁酸叔丁酯、过氧化新戊酸叔丁酯及过氧化氢等过氧化物;2,2’-偶氮双(2-脒基丙烷)二盐酸盐、2,2’-偶氮双[2-(N-苯基脒基)丙烷]二盐酸盐、2,2’-偶氮双[2-(N-烯丙基脒基)丙烷]二盐酸盐、2,2’-偶氮双[2-(2-咪唑啉-2-基)丙烷]二盐酸盐、2,2’-偶氮双{2-[1-(2-羟基乙基)-2-咪唑啉-2-基]丙烷}二盐酸盐、2,2’-偶氮双{2-甲基-N-[1,1-双(羟基甲基)-2-羟基乙基]丙酰胺}、2,2’-偶氮双[2-甲基-N-(2-羟基乙基)-丙酰胺]、4,4’-偶氮双(4-氰基戊酸)等偶氮化合物等。其中,优选过硫酸钾、过硫酸铵、过硫酸钠、2,2’-偶氮双(2-脒基丙烷)二盐酸盐、2,2’-偶氮双[2-(2-咪唑啉-2-基)丙烷]二盐酸盐、2,2’-偶氮双{2-[1-(2-羟基乙基)-2-咪唑啉-2-基]丙烷}二盐酸盐。这些自由基聚合引发剂可以分别单独使用,也可以组合使用两种以上。
相对于1摩尔烯属不饱和单体,自由基聚合引发剂的使用量可以为0.00005~0.01摩尔。若自由基聚合引发剂的使用量为0.00005摩尔以上,则无需长时间进行聚合反应而具有效率。若使用量为0.01摩尔以下,则具有不会发生急剧的聚合反应的倾向。
上述自由基聚合引发剂也能够与亚硫酸钠、亚硫酸氢钠、硫酸亚铁、L-抗坏血酸等还原剂一同使用而用作氧化还原聚合引发剂。
聚合反应时,用于聚合的烯属不饱和单体水溶液可以包含链转移剂。作为链转移剂,例如可列举出次磷酸盐类、硫醇类、硫醇酸类、仲醇类、胺类等。
此外,为了控制吸水性树脂颗粒的粒径,用于聚合的烯属不饱和单体水溶液中可以包含增稠剂。
作为增稠剂,例如能够使用羟乙基纤维素、羟丙基纤维素、甲基纤维素、羧甲基纤维素、聚乙二醇、聚丙烯酰胺、聚乙烯亚胺、糊精、海藻酸钠、聚乙烯醇、聚乙烯吡咯烷酮、聚环氧乙烷等。另外,若聚合时的搅拌速度相同,则具有烯属不饱和单体水溶液的粘度越高,所获得的颗粒的中值粒径越大的倾向。
烃分散介质可以包含选自由碳原子数为6~8的链状脂肪族烃及碳原子数为6~8的脂环族烃组成的组中的至少一种化合物。作为烃分散介质,例如可列举出正己烷、正庚烷、2-甲基己烷、3-甲基己烷、2,3-二甲基戊烷、3-乙基戊烷、正辛烷等链状脂肪族烃;环己烷、甲基环己烷、环戊烷、甲基环戊烷、反式-1,2-二甲基环戊烷、顺式-1,3-二甲基环戊烷、反式-1,3-二甲基环戊烷等脂环族烃;苯、甲苯、二甲苯等芳香族烃等。这些烃分散介质可以单独使用,也可以组合使用两种以上。从工业上容易获得且品质稳定的角度出发,烃分散介质可以包含正庚烷、环己烷或这两者。此外,从同一角度出发,作为上述烃分散介质的混合物,例如可以使用市售的Exxsol Heptane(Exxon Mobil Corporation制造:含有正庚烷及同分异构体的烃75~85%)。
从适度去除聚合热,容易控制聚合温度的角度出发,相对于100质量份的单体水溶液,烃分散介质的使用量优选为30~1000质量份,更优选为40~500质量份,进一步优选为50~300质量份。通过使烃分散介质的使用量为30质量份以上,具有容易控制聚合温度的倾向。通过使烃分散介质的使用量为1000质量份以下,具有聚合的生产率提高的倾向且节省费用。
通常,虽然聚合时会发生基于自交联的内部交联,但也可以通过进一步使用内部交联剂来实施内部交联,并控制吸水性树脂颗粒的吸水特性。作为所使用的内部交联剂,例如可列举出乙二醇、丙二醇、三羟甲基丙烷、甘油、聚氧乙二醇、聚氧丙二醇、聚甘油等多元醇类的二(甲基)丙烯酸酯或三(甲基)丙烯酸酯类;使上述多元醇类与马来酸、富马酸等不饱和酸进行反应而获得的不饱和聚酯类;N,N’-亚甲基双(甲基)丙烯酰胺等双(甲基)丙烯酰胺类;使聚环氧化物与(甲基)丙烯酸进行反应而获得的二(甲基)丙烯酸酯或三(甲基)丙烯酸酯类;使甲苯二异氰酸酯、六亚甲基二异氰酸酯等多异氰酸酯与(甲基)丙烯酸羟乙酯进行反应而获得的二(甲基)丙烯酸氨基甲酰酯类;烯丙基化淀粉、烯丙基化纤维素、邻苯二甲酸二烯丙酯、N,N’,N”-三烯丙基异氰脲酸酯、二乙烯基苯等具有2个以上的聚合性不饱和基团的化合物;(聚)乙二醇二缩水甘油醚、(聚)丙二醇二缩水甘油醚、(聚)甘油二缩水甘油醚、(聚)甘油三缩水甘油醚、(聚)丙二醇聚缩水甘油醚、聚甘油聚缩水甘油醚等聚缩水甘油化合物;环氧氯丙烷、环氧溴丙烷、α-甲基环氧氯丙烷等卤代环氧化合物;2,4-甲苯二异氰酸酯、六亚甲基二异氰酸酯等异氰酸酯化合物等具有2个以上的反应性官能团的化合物等。在这些内部交联剂中,优选使用聚缩水甘油化合物,更优选使用二缩水甘油醚化合物,特别优选使用(聚)乙二醇二缩水甘油醚、(聚)丙二醇二缩水甘油醚、(聚)甘油二缩水甘油醚。这些交联剂可以单独使用,也可以组合使用两种以上。
从通过所获得的聚合物适度交联而抑制水溶性的性质、并显示充分的吸水量的角度出发,相对于每1摩尔烯属不饱和单体,内部交联剂的量优选为0~0.03摩尔,更优选为0.00001~0.01摩尔,进一步优选为0.00002~0.005摩尔。
能够将含有烯属不饱和单体、自由基聚合引发剂、根据需要的内部交联剂等成分的水相、与含有烃类分散介质、根据需要的表面活性剂、高分子类分散剂等成分的油相混合,并在搅拌下进行加热,在油包水体系中进行反相悬浮聚合。
进行反相悬浮聚合时,在表面活性剂、根据需要的高分子类分散剂的存在下,使包含烯属不饱和单体的单体水溶液分散于烃分散介质中。此时,只要是在聚合反应开始之前,则表面活性剂、高分子类分散剂的添加时期可以在添加单体水溶液之前,也可以在添加单体水溶液之后。
其中,从容易降低所获得的吸水性树脂中残留的烃分散介质量的角度出发,优选在使单体水溶液分散于已分散有高分子类分散剂的烃分散介质中之后,进一步使表面活性剂分散,然后进行聚合。
能够以一阶段或两阶段以上的多阶段进行这种反相悬浮聚合。此外,从提高生产率的角度出发,优选以两~三阶段进行。
以两阶段以上的多阶段进行反相悬浮聚合时,在进行第一阶段的反相悬浮聚合之后,向第一阶段的聚合反应中获得的反应混合物中添加烯属不饱和单体并进行混合,并以与第一阶段相同的方法进行第二阶段以后的反相悬浮聚合即可。在第二阶段以后的各阶段的反相悬浮聚合中,优选除了烯属不饱和单体以外,以在第二阶段以后的各阶段的反相悬浮聚合时所添加的烯属不饱和单体的量为基准,在各成分相对于烯属不饱和单体的上述摩尔比范围内,添加上述自由基聚合引发剂或内部交联剂,进行反相悬浮聚合。另外,在第二阶段以后的各阶段的反相悬浮聚合中,根据需要也可以使用内部交联剂。使用内部交联剂时,优选以供于各阶段的烯属不饱和单体的量为基准,在各成分相对于烯属不饱和单体的上述摩尔比范围内添加内部交联剂,进行反相悬浮聚合。
聚合反应的温度根据所使用的自由基聚合引发剂而有所不同,但从通过迅速进行聚合并缩短聚合时间从而提高经济性,且同时容易去除聚合热使反应顺利进行的角度出发,优选为20~150℃,更优选为40~120℃。反应时间通常为0.5~4小时。例如能够通过反应体系内的温度停止上升来确认聚合反应的结束。由此,通常以含水凝胶的状态获得烯属不饱和单体的聚合物。
聚合后,可以通过向所获得的含水凝胶状聚合物中添加交联剂并加热来实施聚合后交联。通过进行聚合后交联,可提高含水凝胶状聚合物的交联度,从而能够更优选地提高吸水特性。
作为用于进行聚合后交联的交联剂,例如可列举出乙二醇、丙二醇、1,4-丁二醇、三羟甲基丙烷、甘油、聚氧乙二醇、聚氧丙二醇、聚甘油等多元醇;(聚)乙二醇二缩水甘油醚、(聚)丙二醇二缩水甘油醚及(聚)甘油二缩水甘油醚等具有2个以上的环氧基的化合物;环氧氯丙烷、环氧溴丙烷及α-甲基环氧氯丙烷等卤代环氧化合物;2,4-甲苯二异氰酸酯及六亚甲基二异氰酸酯等具有2个以上的异氰酸酯基的化合物;1,2-乙烯基双噁唑啉等噁唑啉化合物;碳酸亚乙酯等碳酸酯化合物;双[N,N-二(β-羟基乙基)]己二酰胺等羟基烷基酰胺化合物等。其中,优选(聚)乙二醇二缩水甘油醚、(聚)甘油二缩水甘油醚、(聚)甘油三缩水甘油醚、(聚)丙二醇聚缩水甘油醚、聚甘油聚缩水甘油醚等聚缩水甘油化合物。这些交联剂可以单独使用,也可以组合使用两种以上。
从通过使所获得的含水凝胶状聚合物适度交联而显示适宜的吸水特性的角度出发,相对于每1摩尔烯属不饱和单体,聚合后交联中所使用的交联剂的量优选为0~0.03摩尔,更优选为0~0.01摩尔,进一步优选为0.00001~0.005摩尔。若上述交联剂的添加量在上述范围内,则容易获得减压下的保水率适宜的吸水性树脂颗粒。
作为聚合后交联的添加时期,只要在用于聚合的烯属不饱和单体的聚合后即可,多阶段聚合的情况下,优选在多阶段聚合后添加。另外,考虑到聚合时及聚合后的发热、工序延迟所引起的滞留、添加交联剂时的体系的开放、及伴随交联剂添加而添加水等引起的水分的变动,从含水率(后述)的角度出发,优选在[刚聚合之后的含水率±3质量%]的范围内添加聚合后交联的交联剂。
接着,为了从所获得的含水凝胶状聚合物中去除水分而进行干燥。通过干燥,可获得包含烯属不饱和单体的聚合物的聚合物颗粒。作为干燥方法,例如可列举出:(a)通过在上述含水凝胶状聚合物分散于烃分散介质的状态下,从外部进行加热,从而进行共沸蒸馏,并使烃分散介质回流而去除水分的方法;(b)通过倾析提取含水凝胶状聚合物,并进行减压干燥的方法;及(c)通过过滤器滤除含水凝胶状聚合物,并进行减压干燥的方法等。其中,从制造工序上的简便性出发,优选使用(a)的方法。
例如能够通过调节聚合反应时的搅拌机的转速、或者通过在聚合反应后或干燥初期向体系内添加粉末状无机凝聚剂,从而控制吸水性树脂颗粒的粒径。通过添加凝聚剂,能够增大所获得的吸水性树脂颗粒的粒径。作为粉末状无机凝聚剂的实例,可列举出二氧化硅、沸石、膨润土、氧化铝、滑石、二氧化钛、高岭土、黏土、水滑石等,其中从凝聚效果的角度出发,优选二氧化硅、氧化铝、滑石或高岭土。
在反相悬浮聚合中,作为添加粉末状无机凝聚剂的方法,优选如下方法:预先将粉末状无机凝聚剂分散于与聚合中所使用的烃分散介质同种的烃分散介质或水中,然后混合于搅拌下的包含含水凝胶状聚合物的烃分散介质中。
在本实施方案的吸水性树脂颗粒的制造中,优选在干燥工序或后续的任意工序中,使用交联剂进行含水凝胶状聚合物的表面部分的交联(表面交联)。表面交联优选在含水凝胶状聚合物为特定的含水率的时机进行。表面交联的时期优选为含水凝胶状聚合物的含水率为5~50质量%的时刻,更优选为10~40质量%的时刻,进一步优选为15~35质量%的时刻。
利用下式计算含水凝胶状聚合物的含水率(质量%)。
含水率=[Ww/(Ww+Ws)]×100
Ww:从整个聚合工序的聚合前的水性液中含有的水分量中减去通过干燥工序排出至体系外部的水分量,在该得到的量的基础上加上混合粉末状无机凝聚剂、表面交联剂等时根据需要使用的水分量,由此得到的含水凝胶状聚合物的水分量。
Ws:根据构成含水凝胶状聚合物的烯属不饱和单体、交联剂、引发剂等材料的使用量计算的固体成分量。
作为用于进行表面交联的表面交联剂,可列举出具有2个以上的反应性官能团的化合物。作为其实例,可列举出乙二醇、丙二醇、1,4-丁二醇、三羟甲基丙烷、甘油、聚氧乙二醇、聚氧丙二醇、聚甘油等多元醇类;(聚)乙二醇二缩水甘油醚、(聚)甘油二缩水甘油醚、(聚)甘油三缩水甘油醚、三羟甲基丙烷三缩水甘油醚、(聚)丙二醇聚缩水甘油醚、(聚)甘油聚缩水甘油醚等聚缩水甘油化合物;环氧氯丙烷、环氧溴丙烷、α-甲基环氧氯丙烷等卤代环氧化合物;2,4-甲苯二异氰酸酯、六亚甲基二异氰酸酯等异氰酸酯化合物;3-甲基-3-氧杂环丁烷甲醇、3-乙基-3-氧杂环丁烷甲醇、3-丁基-3-氧杂环丁烷甲醇、3-甲基-3-氧杂环丁烷乙醇、3-乙基-3-氧杂环丁烷乙醇、3-丁基-3-氧杂环丁烷乙醇等氧杂环丁烷化合物;1,2-乙烯基双噁唑啉等噁唑啉化合物;碳酸亚乙酯等碳酸酯化合物;双[N,N-二(β-羟基乙基)]己二酰胺等羟基烷基酰胺化合物。其中,更优选(聚)乙二醇二缩水甘油醚、(聚)甘油二缩水甘油醚、(聚)甘油三缩水甘油醚、(聚)丙二醇聚缩水甘油醚、聚甘油聚缩水甘油醚等聚缩水甘油化合物。这些表面交联剂可以单独使用,也可以组合使用两种以上。
从通过使所获得的含水凝胶状聚合物适度交联而显示适宜的吸水特性的角度出发,通常,相对于1摩尔用于聚合的烯属不饱和单体,表面交联剂的量为0.00001~0.02摩尔,优选为0.00005~0.01摩尔,更优选为0.0001~0.005摩尔的比。
从充分提高吸水性树脂颗粒的表面部分的交联密度、提高吸水性树脂颗粒的凝胶强度的角度出发,表面交联剂的使用量优选为0.00001摩尔以上。此外,从提高减压下的保水率、提高吸水性树脂颗粒的保水能力的角度出发,优选为0.02摩尔以下。
在表面交联反应后,通过公知的方法蒸馏去除水及烃分散介质,从而能够获得作为表面交联后的干燥品的聚合物颗粒。
本实施方案的吸水性树脂颗粒可以仅由聚合物颗粒构成,但例如能够进一步包含选自无机粉末、表面活性剂、氧化剂、还原剂、金属螯合剂(乙二胺四乙酸及其盐、二乙烯三胺五乙酸及其盐、例如二乙烯三胺五乙酸五钠等)、自由基链抑制剂、抗氧化剂、抗菌剂、除臭剂、凝胶稳定剂、流动性改进剂(润滑剂)等中的各种追加成分。追加成分可配置于聚合物颗粒的内部、聚合物颗粒的表面上或聚合物颗粒的内部及表面。作为追加成分,优选流动性改进剂(润滑剂),其中,更优选无机颗粒。作为无机颗粒,例如可列举出无定形二氧化硅等二氧化硅颗粒。例如,通过添加相对于100质量份的聚合物颗粒为0.05~5质量份的作为无机颗粒的无定形二氧化硅,能够提高吸水性树脂颗粒的流动性。
吸水性树脂颗粒可以包含配置于聚合物颗粒的表面上的多个无机颗粒。例如,通过混合聚合物颗粒与无机颗粒,能够在聚合物颗粒的表面上配置无机颗粒。该无机颗粒可以为无定形二氧化硅等二氧化硅颗粒。当吸水性树脂颗粒包含配置于聚合物颗粒的表面上的无机颗粒时,无机颗粒相对于聚合物颗粒的质量的比例可以为0.2质量%以上、0.5质量%以上、1.0质量%以上或1.5质量%以上,也可以为5.0质量%以下或3.5质量%以下。与聚合物颗粒的大小相比,此处的无机颗粒通常具有微小的大小。例如,无机颗粒的平均粒径可以为0.1~50μm、0.5~30μm或1~20μm。此处的平均粒径为能够通过动态光散射法或激光衍射散射法测定的值。通过使无机颗粒的添加量在上述范围内,容易获得吸水特性良好且减压下的保水率适宜的吸水性树脂颗粒。
本实施方案的吸水性树脂颗粒对尿液、血液等体液的吸收性优异,例如,能够应用于纸尿布、卫生巾、卫生棉条等卫生用品;宠物垫、狗或猫的厕所制剂等动物排泄物处理材料等领域。
本实施方案的吸水性树脂颗粒能够适宜用于吸收体。本实施方案的吸收体包含吸水性树脂颗粒。吸收体例如可以进一步具备纤维状物。
相对于吸水性树脂颗粒及纤维状物的合计,吸收体中的吸水性树脂颗粒的质量比例可以为2质量%~100质量%,优选为10质量%~80质量%,更优选为20质量%~70质量%。作为吸收体的结构,例如可以为吸水性树脂颗粒及纤维状物均匀混合的形态,也可以为在形成为片状或层状的纤维状物之间夹有吸水性树脂颗粒的形态,还可以为其他形态。
作为纤维状物,例如可列举出经微粉碎的木浆、棉花、棉绒、人造丝、乙酸纤维素等纤维素类纤维、聚酰胺、聚酯、聚烯烃等合成纤维。此外,纤维状物可以为上述纤维的混合物。
为了提高吸收体在使用前及使用中的形态保持性,可以通过对纤维状物添加粘合性粘结剂而使纤维彼此粘合。作为粘合性粘结剂,例如可列举出热熔接性合成纤维、热熔粘合剂、粘合性乳剂等。
作为热熔接性合成纤维,例如可列举出聚乙烯、聚丙烯、乙烯-丙烯共聚物等全熔型粘结剂、由聚丙烯与聚乙烯的并列或芯鞘结构构成的非全熔型粘结剂。在上述非全熔型粘结剂中,仅聚乙烯部分热熔接。作为热熔粘合剂,例如可列举出乙烯-乙酸乙烯酯共聚物、苯乙烯-异戊二烯-苯乙烯嵌段共聚物、苯乙烯-丁二烯-苯乙烯嵌段共聚物、苯乙烯-乙烯-丁烯-苯乙烯嵌段共聚物、苯乙烯-乙烯-丙烯-苯乙烯嵌段共聚物、非晶态聚丙烯等基础聚合物与增粘剂、增塑剂、抗氧化剂等的掺合物。
作为粘合性乳剂,例如可列举出选自由甲基丙烯酸甲酯、苯乙烯、丙烯腈、丙烯酸2-乙基己酯、丙烯酸丁酯、丁二烯、乙烯及乙酸乙烯酯组成的组中的至少一种以上的单体的聚合物。这些粘合性粘结剂可以单独使用,也可以组合使用两种以上。
本实施方案的吸收体可以进一步包含无机粉末(例如无定形二氧化硅)、除臭剂、抗菌剂、香料等。当吸水性树脂颗粒包含无机颗粒时,吸收体可以包含与吸水性树脂颗粒中的无机颗粒不同的无机粉末。
本实施方案的吸收体的形状并没有特别限定,例如可以为片状。吸收体的厚度(例如,片状吸收体的厚度)例如可以为0.1~20mm、0.3~15mm。
本实施方案的吸收性物品具备本实施方案的吸收体。本实施方案的吸收性物品可列举出保持吸收体的形状的芯包片;配置于吸液对象的液体渗入的一侧的最外部的透液性片;及配置于与吸液对象的液体渗入的一侧为相反侧的最外部的不透液性片等。作为吸收性物品,可列举出尿布(例如纸尿布)、如厕训练裤、失禁垫、卫生用品(卫生巾、卫生棉条等)、吸汗垫、宠物垫、简易马桶用构件、动物排泄物处理材料等。
图1为表示吸收性物品的一个实例的剖面图。图1所示的吸收性物品100具备吸收体10、芯包片20a、20b、透液性片30及不透液性片40。在吸收性物品100中,依次层叠有不透液性片材40、芯包片20b、吸收体10、芯包片20a及透液性片材30。在图1中,存在图示为在部件之间具有间隙的部分,但是部件之间也可以密合,不存在该间隙。
吸收体10具有本实施方案的吸水性树脂颗粒10a及包含纤维状物的纤维层10b。吸水性树脂颗粒10a分散于纤维层10b内。
芯包片20a以与吸收体10相接的状态配置于吸收体10的一侧(图1中,吸收体10的上侧)。芯包片20b以与吸收体10相接的状态配置于吸收体10的另一侧(图1中,吸收体10的下侧)。吸收体10配置于芯包片20a与芯包片20b之间。作为芯包片20a、20b,可列举出纸巾、无纺布等。芯包片20a及芯包片20b例如具有与吸收体10同等大小的主表面。
透液性片30配置于吸收对象的液体所渗入的一侧的最外部。透液性片30以与芯包片20a相接的状态配置于芯包片20a上。作为透液性片30,可列举出由聚乙烯、聚丙烯、聚酯、聚酰胺等合成树脂形成的无纺布、多孔片等。不透液性片40在吸收性物品100中配置在与透液性片30为相反侧的最外部。不透液性片40以与芯包片20b相接的状态配置于芯包片20b的下侧。作为不透液性片40,可列举出由聚乙烯、聚丙烯、聚氯乙烯等合成树脂形成的片、由这些合成树脂与无纺布的复合材料形成的片等。透液性片30及不透液性片40例如具有比吸收体10的主表面大的主表面,透液性片30及不透液性片40的外缘部延伸至吸收体10及芯包片20a、20b的周围。
吸收体10、芯包片20a、20b、透液性片30及不透液性片40的大小关系没有特别限定,可根据吸收性物品的用途等适当调节。此外,使用芯包片20a、20b保持吸收体10的形状的方法没有特别限定,如图1所示,可以利用多片芯包片包裹吸收体,也可以利用一片芯包片包裹吸收体。
实施例
以下列举实施例对本发明进行进一步详细说明,但本发明并不仅限于这些实施例。
[吸水性树脂颗粒的制造]
(实施例1)
准备内径为11cm、容积为2L的圆底圆筒型可拆式烧瓶,其具备回流冷凝器、滴液漏斗、氮气导入管及作为搅拌机的搅拌桨,该搅拌桨具有2层叶片直径为5cm的4片斜浆式叶片。取作为烃分散介质的正庚烷293g于该烧瓶中,添加作为高分子类分散剂的马来酸酐改性乙烯-丙烯共聚物(Mitsui Chemicals,Inc.,Hi-WAX1105A)0.736g,边搅拌边升温至80℃以溶解分散剂,然后冷却至50℃。
另一方面,取作为烯属不饱和单体的80.5质量%的丙烯酸水溶液92.0g(1.03摩尔)于内容积为300mL的烧杯中,从外部进行冷却,同时滴加20.9质量%的氢氧化钠水溶液147.7g,由此进行75摩尔%的中和,然后,加入作为增稠剂的羟乙基纤维素0.092g(SUMITOMO SEIKA CHEMICALS CO.,LTD.,HEC AW-15F)、作为自由基聚合引发剂的过硫酸钾0.0736g(0.272毫摩尔)、作为内部交联剂的乙二醇二缩水甘油醚0.010g(0.057毫摩尔)并使其溶解,制备第一阶段的水性液。
将制备的水性液添加至可拆式烧瓶内,并搅拌10分钟后,进一步添加表面活性剂溶液,该表面活性剂溶液通过使作为表面活性剂的HLB3的蔗糖硬脂酸酯(Mitsubishi-Chemical Foods Corporation,RYOTO SUGAR ESTER S-370)0.736g加热溶解于正庚烷6.62g中而得到,一边将搅拌机的转速设为550rpm进行搅拌一边利用氮气充分对体系内进行置换之后,将烧瓶浸渍于70℃的水浴中升温,进行60分钟的聚合,由此获得第一阶段的聚合浆液。
另一方面,取作为烯属不饱和单体的80.5质量%的丙烯酸水溶液128.8g(1.43摩尔)于另一个内容积为500mL的烧杯中,从外部进行冷却,同时滴加27质量%的氢氧化钠水溶液159.0g,由此进行75摩尔%的中和,然后,加入作为自由基聚合引发剂的过硫酸钾0.090g(0.334毫摩尔)并使其溶解,制备第二阶段的水性液。
一边将搅拌机的转速设为1000rpm进行搅拌,一边将上述可拆式烧瓶体系内冷却至25℃之后,将上述第二阶段的水性液全部添加到第一阶段的聚合浆液中,利用氮气对体系内进行30分钟置换之后,再次将烧瓶浸渍于70℃的水浴中升温,进行60分钟的聚合反应。聚合后,添加作为交联剂的2质量%的乙二醇二缩水甘油醚0.580g(0.067毫摩尔),获得含水凝胶状聚合物。
在搅拌下,将45质量%的二乙烯三胺五乙酸五钠水溶液0.265g添加到第二阶段的聚合后的含水凝胶状聚合物中。然后,将烧瓶浸渍于设定为125℃的油浴中,通过正庚烷与水的共沸蒸馏,一边使正庚烷回流,一边向体系外抽出256.1g的水。然后,在烧瓶中,添加作为表面交联剂的2质量%的乙二醇二缩水甘油醚水溶液4.42g(0.507毫摩尔),并在83℃下保持2小时。
然后,通过在125℃下使正庚烷蒸发并干燥而获得干燥品(聚合物颗粒)。使该干燥品通过孔径850μm的筛,且将0.2质量%的无定形二氧化硅(Oriental SilicasCorporation,Tokusil NP-S)与干燥品混合,获得230.8g吸水性树脂颗粒。该颗粒的中值粒径为349μm。
(实施例2)
准备内径为11cm、容积为2L的圆底圆筒型可拆式烧瓶,其具备回流冷凝器、滴液漏斗、氮气导入管及作为搅拌机的搅拌桨,该搅拌桨具有2层叶片直径为5cm的4片斜浆式叶片。取作为烃分散介质的正庚烷293g于该烧瓶中,添加作为高分子类分散剂的马来酸酐改性乙烯-丙烯共聚物(Mitsui Chemicals,Inc.,Hi-WAX1105A)0.736g,边搅拌边升温至80℃以溶解分散剂,然后冷却至50℃。
另一方面,取作为烯属不饱和单体的80.5质量%的丙烯酸水溶液92.0g(1.03摩尔)于内容积为300mL的烧杯中,从外部进行冷却,同时滴加20.9质量%的氢氧化钠水溶液147.7g,由此进行75摩尔%的中和,然后,加入作为增稠剂的羟乙基纤维素0.092g(SUMITOMO SEIKA CHEMICALS CO.,LTD.,HEC AW-15F)、作为自由基聚合引发剂的过硫酸钾0.0736g(0.272毫摩尔)、作为内部交联剂的乙二醇二缩水甘油醚0.010g(0.057毫摩尔)并使其溶解,制备第一阶段的水性液。
将制备的水性液添加至可拆式烧瓶内,并搅拌10分钟后,进一步添加表面活性剂溶液,该表面活性剂溶液通过使作为表面活性剂的HLB3的蔗糖硬脂酸酯(Mitsubishi-Chemical Foods Corporation,RYOTO SUGAR ESTER S-370)0.736g加热溶解于正庚烷6.62g中而得到,一边将搅拌机的转速设为550rpm进行搅拌一边利用氮气充分对体系内进行置换之后,将烧瓶浸渍于70℃的水浴中升温,进行60分钟的聚合,由此获得第一阶段的聚合浆液。
另一方面,取作为烯属不饱和单体的80.5质量%的丙烯酸水溶液128.8g(1.43摩尔)于另一个内容积为500mL的烧杯中,从外部进行冷却,同时滴加27质量%的氢氧化钠水溶液159.0g,由此进行75摩尔%的中和,然后,加入作为自由基聚合引发剂的过硫酸钾0.090g(0.334毫摩尔)并使其溶解,制备第二阶段的水性液。
一边将搅拌机的转速设为1000rpm进行搅拌,一边将上述可拆式烧瓶体系内冷却至25℃之后,将上述第二阶段的水性液全部添加到第一阶段的聚合浆液中,利用氮气对体系内进行30分钟置换之后,再次将烧瓶浸渍于70℃的水浴中升温,进行60分钟的聚合反应。聚合后,添加作为交联剂的2质量%的乙二醇二缩水甘油醚0.580g(0.067毫摩尔),获得含水凝胶状聚合物。
在搅拌下,将45质量%的二乙烯三胺五乙酸五钠水溶液0.265g添加到第二阶段的聚合后的含水凝胶状聚合物中。然后,将烧瓶浸渍于设定为125℃的油浴中,通过正庚烷与水的共沸蒸馏,一边使正庚烷回流,一边向体系外抽出272.5g的水。然后,在烧瓶中,添加作为表面交联剂的2质量%的乙二醇二缩水甘油醚水溶液4.42g(0.507毫摩尔),并在83℃下保持2小时。
然后,通过在125℃下使正庚烷蒸发并干燥而获得干燥品(聚合物颗粒)。使该干燥品通过孔径850μm的筛,且将0.2质量%的无定形二氧化硅(Oriental SilicasCorporation,Tokusil NP-S)与干燥品混合,获得228.8g的吸水性树脂颗粒。该颗粒的中值粒径为359μm。
(实施例3)
准备内径为11cm、容积为2L的圆底圆筒型可拆式烧瓶,其具备回流冷凝器、滴液漏斗、氮气导入管及作为搅拌机的搅拌桨,该搅拌桨具有2层叶片直径为5cm的4片斜浆式叶片。取作为烃分散介质的正庚烷293g于该烧瓶中,添加作为高分子类分散剂的马来酸酐改性乙烯-丙烯共聚物(Mitsui Chemicals,Inc.,Hi-WAX1105A)0.736g,边搅拌边升温至80℃以溶解分散剂,然后冷却至50℃。
另一方面,取作为烯属不饱和单体的80.5质量%的丙烯酸水溶液92.0g(1.03摩尔)于内容积为300mL的烧杯中,从外部进行冷却,同时滴加20.9质量%的氢氧化钠水溶液147.7g,由此进行75摩尔%的中和,然后,加入作为增稠剂的羟乙基纤维素0.092g(SUMITOMO SEIKA CHEMICALS CO.,LTD.,HEC AW-15F)、作为自由基聚合引发剂的过硫酸钾0.0736g(0.272毫摩尔)、作为内部交联剂的乙二醇二缩水甘油醚0.010g(0.057毫摩尔)并使其溶解,制备第一阶段的水性液。
将制备的水性液添加至可拆式烧瓶内,并搅拌10分钟后,进一步添加表面活性剂溶液,该表面活性剂溶液通过使作为表面活性剂的HLB3的蔗糖硬脂酸酯(Mitsubishi-Chemical Foods Corporation,RYOTO SUGAR ESTER S-370)0.736g加热溶解于正庚烷6.62g中而得到,一边将搅拌机的转速设为550rpm进行搅拌一边利用氮气充分对体系内进行置换之后,将烧瓶浸渍于70℃的水浴中升温,进行60分钟的聚合,由此获得第一阶段的聚合浆液。
另一方面,取作为烯属不饱和单体的80.5质量%的丙烯酸水溶液128.8g(1.43摩尔)于另一个内容积为500mL的烧杯中,从外部进行冷却,同时滴加27质量%的氢氧化钠水溶液159.0g,由此进行75摩尔%的中和,然后,加入作为自由基聚合引发剂的过硫酸钾0.090g(0.334毫摩尔)并使其溶解,制备第二阶段的水性液。
一边将搅拌机的转速设为1000rpm进行搅拌,一边将上述可拆式烧瓶体系内冷却至25℃之后,将上述第二阶段的水性液全部添加到第一阶段的聚合浆液中,利用氮气对体系内进行30分钟置换之后,再次将烧瓶浸渍于70℃的水浴中升温,进行60分钟的聚合反应。聚合后,添加作为交联剂的2质量%的乙二醇二缩水甘油醚0.580g(0.067毫摩尔),获得含水凝胶状聚合物。
在搅拌下,将45质量%的二乙烯三胺五乙酸五钠水溶液0.265g添加到第二阶段的聚合后的含水凝胶状聚合物中。然后,将烧瓶浸渍于设定为125℃的油浴中,通过正庚烷与水的共沸蒸馏,一边使正庚烷回流,一边向体系外抽出247.9g的水。然后,在烧瓶中,添加作为表面交联剂的2质量%的乙二醇二缩水甘油醚水溶液4.42g(0.507毫摩尔),并在83℃下保持2小时。
然后,通过在125℃下使正庚烷蒸发并干燥而获得干燥品(聚合物颗粒)。使该干燥品通过孔径850μm的筛,且将0.2质量%的无定形二氧化硅(Oriental SilicasCorporation,Tokusil NP-S)与干燥品混合,获得231.0g的吸水性树脂颗粒。该颗粒的中值粒径为357μm。
(实施例4)
准备内径为11cm、容积为2L的圆底圆筒型可拆式烧瓶,其具备回流冷凝器、滴液漏斗、氮气导入管及作为搅拌机的搅拌桨,该搅拌桨具有2层叶片直径为5cm的4片斜浆式叶片。取作为烃分散介质的正庚烷293g于该烧瓶中,添加作为高分子类分散剂的马来酸酐改性乙烯-丙烯共聚物(Mitsui Chemicals,Inc.,Hi-WAX1105A)0.736g,边搅拌边升温至80℃以溶解分散剂,然后冷却至50℃。
另一方面,取作为烯属不饱和单体的80.5质量%的丙烯酸水溶液92.0g(1.03摩尔)于内容积为300mL的烧杯中,从外部进行冷却,同时滴加20.9质量%的氢氧化钠水溶液147.7g,由此进行75摩尔%的中和,然后,加入作为增稠剂的羟乙基纤维素0.092g(SUMITOMO SEIKA CHEMICALS CO.,LTD.,HEC AW-15F)、作为自由基聚合引发剂的2,2’-偶氮双(2-脒基丙烷)二盐酸盐0.092g(0.339毫摩尔)及过硫酸钾0.018g(0.068毫摩尔)、作为内部交联剂的乙二醇二缩水甘油醚0.005g(0.029毫摩尔)并使其溶解,制备第一阶段的水性液。
将制备的水性液添加至可拆式烧瓶内,并搅拌10分钟后,进一步添加表面活性剂溶液,该表面活性剂溶液通过使作为表面活性剂的HLB3的蔗糖硬脂酸酯(Mitsubishi-Chemical Foods Corporation,RYOTO SUGAR ESTER S-370)0.736g加热溶解于正庚烷6.62g中而得到,一边将搅拌机的转速设为550rpm进行搅拌一边利用氮气充分对体系内进行置换之后,将烧瓶浸渍于70℃的水浴中升温,进行60分钟的聚合,由此获得第一阶段的聚合浆液。
另一方面,取作为烯属不饱和单体的80.5质量%的丙烯酸水溶液128.8g(1.43摩尔)于另一个内容积为500mL的烧杯中,从外部进行冷却,同时滴加27质量%的氢氧化钠水溶液159.0g,由此进行75摩尔%的中和,然后,加入作为自由基聚合引发剂的2,2’-偶氮双(2-脒基丙烷)二盐酸盐0.129g(0.475毫摩尔)及过硫酸钾0.026g(0.095毫摩尔)并使其溶解,制备第二阶段的水性液。
一边将搅拌机的转速设为1000rpm进行搅拌,一边将上述可拆式烧瓶体系内冷却至25℃之后,将上述第二阶段的水性液全部添加到第一阶段的聚合浆液中,利用氮气对体系内进行30分钟置换之后,再次将烧瓶浸渍于70℃的水浴中升温,进行60分钟的聚合反应。聚合后,添加作为交联剂的2质量%的乙二醇二缩水甘油醚水溶液0.580g(0.067毫摩尔),获得含水凝胶状聚合物。
在搅拌下,将45质量%的二乙烯三胺五乙酸五钠水溶液0.265g添加到第二阶段的聚合后的含水凝胶状聚合物中。然后,将烧瓶浸渍于设定为125℃的油浴中,通过正庚烷与水的共沸蒸馏,一边使正庚烷回流,一边向体系外抽出234.2g的水。然后,在烧瓶中,添加作为表面交联剂的2质量%的乙二醇二缩水甘油醚水溶液4.42g(0.507毫摩尔),并在83℃下保持2小时。
然后,通过在125℃下使正庚烷蒸发并干燥而获得干燥品(聚合物颗粒)。使该干燥品通过孔径850μm的筛,且将0.2质量%的无定形二氧化硅(Oriental SilicasCorporation,Tokusil NP-S)与干燥品混合,获得231.1g的吸水性树脂颗粒。该颗粒的中值粒径为355μm。
(比较例1)
将从日本销售的Daio Paper Corporation的尿布“GOO.N纸尿裤、全新舒爽透气、男童用L码”采集的吸水性树脂颗粒作为比较例1。该颗粒的中值粒径为403μm。
(比较例2)
准备内径为11cm、容积为2L的带4处侧壁挡板的圆底圆筒型可拆式烧瓶(挡板宽度:7mm),其具备回流冷凝器、滴液漏斗、氮气导入管及作为搅拌机的搅拌桨,该搅拌桨具有2层叶片直径为5cm的4片斜浆式叶片(用氟树脂进行了表面处理)。取作为烃分散介质的正庚烷451g于该烧瓶中,添加作为表面活性剂的HLB8.6的山梨糖醇酐单月桂酸酯(NOFCORPORATION,Nonion LP-20R)0.984g,将搅拌机的转速设为300rpm,并加热至50℃。通过加热,使山梨糖醇酐单月桂酸酯溶解于正庚烷之后,将内温冷却至40℃。
另一方面,向500ml容积的三角烧瓶中加入80.5质量%的丙烯酸水溶液92.0g(1.03摩尔),一边从外部进行冰冷却,一边滴加20.9质量%氢氧化钠水溶液147.7g,由此进行75摩尔%的中和。接着,向所获得的丙烯酸部分中和物水溶液中添加作为自由基聚合引发剂的过硫酸钾0.101g(0.374毫摩尔)并使其溶解,制备单体水溶液。
将上述单体水溶液添加至上述可拆式烧瓶中,利用氮气充分对体系内进行置换之后,将搅拌机的转速设为700rpm,将烧瓶浸渍于70℃的水浴中,并保持60分钟。
然后,将搅拌机的转速设为1000rpm,向包含所生成的含水凝胶状聚合物、正庚烷及表面活性剂的聚合液中,添加预先使作为粉末状无机凝聚剂的无定形二氧化硅(Oriental Silicas Corporation,Tokusil NP-S)0.092g分散于正庚烷100g中而得到的溶液,并混合10分钟。然后,将包含反应液的烧瓶浸渍于125℃的油浴中,通过正庚烷与水的共沸蒸馏,一边使正庚烷回流,一边向体系外抽出112g的水之后,添加作为表面交联剂的乙二醇二缩水甘油醚的10质量%水溶液4.97g(2.85毫摩尔),并在内温80±2℃下保持2小时。
然后,使水及正庚烷蒸发,并干燥到从体系内几乎不再蒸馏出蒸发物之后,暂时从油浴取出烧瓶,用喷雾器将13.8g水以每秒0.3g的流量进行喷雾。然后,一边以每分钟200ml的流量向体系内吹入氮气,一边在80℃下保持30分钟,获得干燥品(聚合物颗粒)。使该干燥品通过孔径为850μm的筛,获得吸水性树脂颗粒90.5g。该颗粒的中值粒径为356μm。
(比较例3)
准备内径为11cm、容积为2L的圆底圆筒型可拆式烧瓶,其具备回流冷凝器、滴液漏斗、氮气导入管及作为搅拌机的搅拌桨,该搅拌桨具有2层叶片直径为5cm的4片斜浆式叶片。取作为烃分散介质的正庚烷293g于该烧瓶中,添加作为高分子类分散剂的马来酸酐改性乙烯-丙烯共聚物(Mitsui Chemicals,Inc.,Hi-WAX1105A)0.736g,边搅拌边升温至80℃以溶解分散剂,然后冷却至50℃。
另一方面,取作为烯属不饱和单体的80.5质量%的丙烯酸水溶液92.0g(1.03摩尔)于内容积为300mL的烧杯中,从外部进行冷却,同时滴加20.9质量%的氢氧化钠水溶液147.7g,由此进行75摩尔%的中和,然后,加入作为增稠剂的羟乙基纤维素0.092g(SUMITOMO SEIKA CHEMICALS CO.,LTD.,HEC AW-15F)、作为自由基聚合引发剂的2,2’-偶氮双(2-脒基丙烷)二盐酸盐0.092g(0.339毫摩尔)及过硫酸钾0.018g(0.068毫摩尔)、作为内部交联剂的乙二醇二缩水甘油醚0.0046g(0.026毫摩尔)并使其溶解,制备第一阶段的水性液。
将制备的水性液添加至可拆式烧瓶内,并搅拌10分钟后,进一步添加表面活性剂溶液,该表面活性剂溶液通过使作为表面活性剂的HLB3的蔗糖硬脂酸酯(Mitsubishi-Chemical Foods Corporation,RYOTO SUGAR ESTER S-370)0.736g加热溶解于正庚烷6.62g中而得到,一边将搅拌机的转速设为550rpm进行搅拌一边利用氮气充分对体系内进行置换之后,将烧瓶浸渍于70℃的水浴中升温,进行60分钟的聚合,由此获得第一阶段的聚合浆液。
另一方面,取作为烯属不饱和单体的80.5质量%的丙烯酸水溶液128.8g(1.43摩尔)于另一个内容积为500mL的烧杯中,从外部进行冷却,同时滴加27质量%的氢氧化钠水溶液159.0g,由此进行75摩尔%的中和,然后,加入作为自由基聚合引发剂的2,2’-偶氮双(2-脒基丙烷)二盐酸盐0.129g(0.475毫摩尔)及过硫酸钾0.026g(0.095毫摩尔)、作为内部交联剂的乙二醇二缩水甘油醚0.0116g(0.067毫摩尔)并使其溶解,制备第二阶段的水性液。
一边将搅拌机的转速设为1000rpm进行搅拌,一边将上述可拆式烧瓶体系内冷却至25℃之后,将上述第二阶段的水性液全部添加到第一阶段的聚合浆液中,利用氮气对体系内进行30分钟置换之后,再次将烧瓶浸渍于70℃的水浴中升温,进行60分钟的聚合反应。
在搅拌下,将45质量%的二乙烯三胺五乙酸五钠水溶液0.265g添加到第二阶段的聚合后的含水凝胶状聚合物中。然后,将烧瓶浸渍于设定为125℃的油浴中,通过正庚烷与水的共沸蒸馏,一边使正庚烷回流,一边向体系外抽出219.2g的水。然后,在烧瓶中,添加作为表面交联剂的2质量%的乙二醇二缩水甘油醚水溶液6.62g(0.761毫摩尔),并在83℃下保持2小时。
然后,通过在125℃下使正庚烷蒸发并干燥而获得干燥品(聚合物颗粒)。使该干燥品通过孔径850μm的筛,且将0.2质量%的无定形二氧化硅(Oriental SilicasCorporation,Tokusil NP-S)与干燥品混合,获得229.6g吸水性树脂颗粒。该颗粒的中值粒径为356μm。
针对所获得的吸水性树脂颗粒,通过以下方法对减压6小时后的保水率、生理盐水保水量、中值粒径及闷热性进行评价。
[减压6小时后的保水率]
在温度25±2℃的室内,边利用磁力搅拌器(无环)以600rpm搅拌放入100mL烧杯内的生理盐水38g,边投入吸水性树脂颗粒2g,且从因搅拌引起的旋涡消失的时刻起,利用市售的包片材料盖住烧杯上部,在25℃下静置30分钟,获得溶胀凝胶。将NIPPON PAPER PAPYLIA CO.,LTD.制造的Heat Pac(MWA18:18gsm,120mm×200mm)对折,制作将除了折痕外的三个边中的两个边被热封的120mm×100mm的茶包,并测定皮重(空茶包)质量。使用刮铲(spatula)将上述溶胀凝胶20.0g装填于上述茶包中后,通过热封封袋而作为评价样品,并立即测定初始评价样品质量。在任一例子中,初始溶胀凝胶量均为20.0g,因此将评价样品中的吸水性树脂颗粒(干燥)质量视为1.0g,进行下述保水率的计算。
将置于孔径38μm的筛上的上述评价样品放入设定为35℃的真空干燥机(AS ONECORPORATION,AS ONE VACUUM OVEN AVO-310N),且使用泵(隔膜型干式真空泵,DTU-20,ULVAC KIKO,Inc.制造)进行排气,将内压设为0.2kPa。使用数字压力计(真空计)DM-10S(SIBATA SCIENTIFIC TECHNOLOGY LTD.制造)测定内压。
每1小时反复进行从真空干燥机取出评价样品并迅速测定质量的操作。通过以下计算式,计算出初始及减压6小时后的溶胀凝胶量、以及减压6小时后的保水率。将结果示于表1。
溶胀凝胶量[g/g]=(评价样品质量[g]-皮重(茶包)质量[g])/评价样品中的吸水性树脂颗粒(干燥)质量[g]
减压6小时后的保水率[%]=(减压6小时后的溶胀凝胶量[g/g]/初始溶胀凝胶量[g/g])×100
[生理盐水保水量]
将称取了吸水性树脂颗粒2.0g的棉袋(阔幅棉布60号,宽100mm×长200mm)设置在500mL容积的烧杯内。向装有吸水性树脂颗粒的棉袋中以不产生结块的方式一次性注入0.9质量%氯化钠水溶液(生理盐水)500g,用橡皮筋绑住棉袋的上部,静置30分钟,从而使吸水性树脂颗粒溶胀。利用离心力设定为167G的脱水机(KOKUSAN Co.Ltd.制造,产品型号:H-122),将经过30分钟后的棉袋脱水1分钟,并测定包含脱水后的溶胀凝胶的棉袋的质量Wa(g)。不添加吸水性树脂颗粒而进行相同操作,测定棉袋湿润时的空质量Wb(g),并由下式计算出生理盐水保水量。
生理盐水保水量(g/g)=[Wa-Wb]/2.0
[中值粒径(粒度分布)]
将吸水性树脂颗粒50g用于测定中值粒径(粒度分布)。
将JIS标准筛从上至下依次以下述顺序组合:孔径850μm的筛、孔径500μm的筛、孔径425μm的筛、孔径300μm的筛、孔径250μm的筛、孔径180μm的筛、孔径150μm的筛及托盘。
在所组合的最上侧的筛放入吸水性树脂颗粒,并利用Ro-Tap型振动器振荡20分钟而进行分级。分级后,将残留在各筛上的吸水性树脂颗粒的质量以相对于总量的质量百分比的形式算出,求出粒度分布。关于该粒度分布,从粒径大的开始依次对筛上进行累计,将筛的孔径与残留在筛上的吸水性树脂颗粒的质量百分比的累计值的关系标绘在对数概率纸上。以直线连接概率纸上的标绘点,并将相当于累计质量百分比为50质量%的粒径作为中值粒径。
[闷热性试验]
将吸水性树脂颗粒1g均匀撒在塑料皿(直径90mm×高度20mm)上,滴加被调节至25±1℃的生理盐水19g,在25±2℃的室内盖住塑料皿并静置30分钟,制作溶胀凝胶。
将装有上述溶胀凝胶的上述塑料皿及温湿度SD数据记录器(AD-5696,A&DCompany,Limited制造)装入泰德拉采样袋(Sansyo Co.,Ltd.制造5L尺寸)内,取下塑料皿的盖之后,利用热封封袋。用软管连接玻璃制200ml注射筒的前端部与泰德拉采样袋的旋塞部,并用上述注射筒反复抽吸,去除采样袋内部的空气,直至内部的皿不移动。使3L干燥空气通过填充在直径10cm、高度20cm的圆筒型容器中的活性炭,并关闭采样袋的旋塞,获得评价样品。另外,对未放入溶胀凝胶的空采样袋同样地进行处理并测定相对湿度,结果为38.8%。将上述评价样品放入35℃的恒温恒湿箱(LHU-113,ESPEC CORP.制造)内,并远程测定10分钟后采样袋内的湿度。将结果示于表1。
[表1]
减压6小时后的保水率充分高的实施例的吸水性树脂颗粒在闷热性试验中的10分后的相对湿度明显低于比较例的吸水性树脂颗粒,表明具有不易闷热的性质。
附图标记说明
10:吸收体;10a:吸水性树脂颗粒;10b:纤维层;20a、20b:芯包片;30:透液性片;40:不透液性片;100:吸收性物品。
Claims (4)
1.一种吸水性树脂颗粒,其包含具有源自烯属不饱和单体的结构单元的交联聚合物,所述烯属不饱和单体包含选自由(甲基)丙烯酸及其盐组成的组中的至少一种化合物,其中,相对于所述交联聚合物中的单体单元总量,(甲基)丙烯酸及其盐的比例为70~100摩尔%,在通过下述测定方法进行的减压下水分保持试验中,保水率6小时值为55质量%以上,生理盐水保水量为32~70g/g,
向在100ml烧杯内以600rpm进行搅拌的生理盐水38g中投入吸水性树脂颗粒2g,且从旋涡消失的时刻起在25℃下静置30分钟,制作溶胀凝胶,将所述溶胀凝胶20g放入12cm×10cm的EDANA WSP241.2R3(12)中规定的无纺布制的茶包内,封袋后作为评价样品,测定质量,将放置在筛上的所述评价样品置于35℃、内压0.2kPa的真空干燥机内,并每1小时测定所述评价样品的质量,
溶胀凝胶量(g/g)=(评价样品质量(g)-皮重(g))/所测定的溶胀凝胶中包含的吸水性树脂颗粒干燥质量(g)
保水率(%)=(减压后溶胀凝胶量(g/g)/初始溶胀凝胶量(g/g))×100。
2.一种吸收体,其含有权利要求1所述的吸水性树脂颗粒。
3.一种吸收性物品,其具备权利要求2所述的吸收体。
4.根据权利要求3所述的吸收性物品,其为尿布。
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