CN108659434A - 吸水性树脂及其制造方法 - Google Patents
吸水性树脂及其制造方法 Download PDFInfo
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- CN108659434A CN108659434A CN201710282424.5A CN201710282424A CN108659434A CN 108659434 A CN108659434 A CN 108659434A CN 201710282424 A CN201710282424 A CN 201710282424A CN 108659434 A CN108659434 A CN 108659434A
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- water
- absorbing resins
- inorganic salts
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- siliceous inorganic
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Abstract
一种吸水性树脂及其制造方法,该吸水性树脂包括树脂颗粒、表面交联剂以及含硅无机盐类颗粒。其中,各树脂颗粒具有内部交联结构,表面交联剂键结于各树脂颗粒的表面,且含硅无机盐类颗粒覆盖住各树脂颗粒的表面。
Description
技术领域
本发明关于一种吸水性树脂及其制造方法,特别是关于一种树脂表面被无机物修饰的吸水性树脂及其制造方法。
背景技术
吸水性树脂广泛地运用于农业或园艺方面的水保持剂、建筑材料中的抗露珠凝结剂以及移除石油中水分的材料,或是电缆线中的外层防水包覆剂以及卫生用品如尿布、妇女卫生用品、抛弃式的擦巾等,尤其使用于尿布上最为大宗。
功能型纸尿裤为目前主要的发展方向,尤其是成人纸尿裤,除强调吸收能力及干爽性外,更朝向具抑菌及除臭能力。基于此种需求,积极进行各种研究,开发具有抑菌及除臭能力并维持吸水特性的吸水性树脂。
常用抑菌或除臭能力的方法是使用沸石颗粒分散于吸水性树脂的内部使其具备除臭能力(美国专利5,980,879号),该专利中公开添加沸石颗粒于重合反应中,使吸水性树脂具备除臭能力,但由于沸石添加量至少约25%,所以大幅降低吸水性树脂的吸收能力;美国公开专利申请20150290052号利用活性碳或沸石颗粒添加于纸尿裤吸收体中,同样具备除臭能力,但上述颗粒会有泄漏于生产设备,甚至于悬浮于厂房空气中,对现场人员健康造成一定程度的伤害。
WO2009/048145公开了一种吸水性树脂的制备方法,添加竹萃取物或茶叶萃取物于吸水性树脂表面或是重合反应中,但是,由于萃取物会影响重合反应,不仅会降低吸水性树脂的吸收能力,而且也会使吸水性树脂的残存单体提高,使接触皮肤时造成红肿现象。此外,使用美国公开专利20030004479号及美国公开专利20040048955号中所提出,将竹或茶粉碎后的粉末,添加于吸水性树脂表面,由于竹或茶粉碎后的粉末分散性低,不易与吸水性树脂混合均一,导致抑菌及除臭能力不佳。
另外,使用活性碳或纳米银离子或沸石表面涂覆银离子,也可以降低臭味或细菌生长现象的发生(美国专利6,663,949号、欧洲专利EP1404385及美国专利7,868,075号),欧洲专利EP 1275404号公开了使用环糊精或是衍生物与吸水性树脂进行混合,以降低臭味的发生,此外,美国公开专利申请20150306272号公开对1,2癸二醇与吸水性树脂进行热处理,以降低臭味的发生。但是,上述方法均无法同时具有抑菌及除臭能力,且只对氨气有较佳的抑制能力。
WO2003/028778公开了调降吸水性树脂的pH值以制备具抑菌的吸水性树脂,美国公开专利申请20010053807号公开了添加氨基乙酸可降低臭味的发生,但经由上述方式所得的吸水性树脂压力下耐尿能力不佳。
日本专利申请1995-165981号公开了具有吸水性树脂和具有磷酸盐化合物的混合物,日本专利申请1999-116829号公开了将吸水性树脂与硅酸盐化合物进行混合,可以提高吸水性树脂的抑菌能力,然而却会降低压力下吸收倍率。
美国专利8,658,146号公开使用单宁(Gallotannin)及其衍生物与吸水性树脂混合,其虽然可以产生出具消臭能力的吸水性树脂,但是,由于成本高且吸水性树脂于高温高湿度的条件下,会有形成黄色或褐色的问题,不适合长期保存。
有鉴于此,仍有必要提供一种同时具有抑菌及除臭能力,而且不会降低吸水特性的吸水性树脂,以解决存在于现有吸水性树脂的缺陷。
发明内容
本发明的目的在于提供一种吸水性树脂及其制造方法,以解决现有技术中吸水性树脂同时具有抑菌及除臭能力时,吸水特性不强的缺陷。
根据本发明的实施例,提供一种吸水性树脂,该吸水性树脂包括多个树脂颗粒、一表面交联剂以及多个含硅无机盐类颗粒。其中,各树脂颗粒具有内部交联结构,表面交联剂键结于各树脂颗粒的表面,且该多个含硅无机盐类颗粒覆盖住各树脂颗粒的表面。
根据本发明的另一实施例,提供一种吸水性树脂的制造方法,其包括:提供酸基单体水溶液,并进行自由基聚合反应,以制得具有内部交联结构的吸水性树脂;切碎吸水性树脂,以获得多个吸水性树脂颗粒;添加表面交联剂于各吸水性树脂颗粒的表面,并进行热处理;以及将含有多个含硅无机盐类颗粒的水溶液涂覆于各吸水性树脂颗粒的表面。
根据本发明的另一实施例,上述各树脂颗粒借由具有不饱和双键的亲水性单体聚合而成。
根据本发明的另一实施例,上述各含硅无机盐类颗粒的组成包括氧化铝及二氧化硅。
根据本发明的另一实施例,上述各含硅无机盐类颗粒中氧化铝及二氧化硅间的重量比介于0.7至0.95。
根据本发明的另一实施例,上述各含硅无机盐类颗粒的粒径介于1-10um。
根据本发明的另一实施例,上述各含硅无机盐类颗粒的组成为高岭土。
根据本发明的另一实施例,上述含有多个含硅无机盐类颗粒的水溶液的pH值介于4-6.5间。
根据本发明的另一实施例,上述含有多个含硅无机盐类颗粒的水溶液和多个吸水性树脂颗粒间的重量百分比介于0.5%至20%。
本发明实施例所提供的吸水性树脂同时具有抑菌及除臭能力,而且仍具有一定的吸水特性。进一步来说,本发明实施例所制造的吸水性树脂对合成尿液具有良好的吸收特性,同时具备优异的抑菌及除臭功能,并且生产时不会造成颗粒泄漏于生产设备,甚至于悬浮于厂房空气,因此可有效降低伤害人员呼吸道的风险。
具体实施方式
于下文中,加以陈述吸水性树脂及其制造方法的具体实施方式,以使本技术领域中普通技术人员可据以实施本发明。虽然本发明的实施例公开如下,然而其并非用以限定本发明,任何熟习此技艺者,在不脱离本发明的精神和范畴内,当可作些许的更动与润饰。
根据本发明的一实施例,提供一种吸水性树脂的制造方法,以制得同时具有抑菌及除臭能力,而且不会降低吸水特性的吸水性树脂。以下就本发明实施例的吸水性树脂的制造方法加以描述。
根据本发明的一实施例,提供一种吸水性树脂的制造方法,所述制造方法至少包括:提供中和率45摩尔百分比以上的水溶性不饱和单体水溶液,例如含酸基单体水溶液。之后,将含酸基单体溶液与聚合反应引发剂进行自由基聚合反应,以形成具有相应组成的水凝胶体。继以将水凝胶体剪切成小水凝胶体。之后,再将上述凝胶体以温度100℃至250℃热风依序进行干燥、粉碎及筛选,以得到吸水性树脂。后续在吸水性树脂的表面进行表面交联反应。在交联反应之后,再添加含有弱酸性含硅化合物的水溶液,以对吸水性树脂进行表面处理。
上述的水溶性不饱和单体可以选自具有酸性基团的不饱和双键的水溶性单体,例如:丙烯酸、甲基丙烯酸、马林酸、富马酸、2-丙烯胺-2-甲基丙烷磺酸、顺丁烯二酸、顺丁烯二酸酐、反丁烯二酸、反丁烯二酸酐等。单体选用不特定限制只可使用一种,也可合并多种单体一齐使用。此外,也可视情况需要添加具有不饱和双键的其他亲水性的单体,例如:丙烯酰胺、甲基丙烯酰胺、丙烯酸-2-羧基乙酯、甲基丙烯酸-2-羧基乙酯、丙烯酸甲酯、丙烯酸乙酯、二甲胺丙烯酰胺、氯化丙烯酰胺基三甲铵,但添加量以不破坏吸水性树脂的物性为原则。
在进行自由基聚合反应时,单体水溶液浓度并没有特别的限制,较佳而言,单体在整体水溶液中的重量百分比应控制在20%至55%之间,更佳浓度为30%至45%之间。当重量百分比浓度在20%以下时,聚合后水凝胶太软且有黏性不利机械加工,但当单体浓度高于55%重量百分比浓度时,单体浓度接近饱和浓度,不仅不易调配,且反应太快,致使反应热不易控制。不饱和单体水溶液的pH值较佳不低于5.5。当pH低于5.5时,会造成聚合后的水凝胶体内残存过多的单体,导致吸水性树脂的物性不佳。
在进行自由基聚合反应前,可添加水溶性高分子于单体水溶液中,以降低成本。上述水溶性高分子可以选自:部份皂化或完全皂化的聚乙烯醇、聚乙二醇、聚丙烯酸、聚丙烯酰胺、淀粉、淀粉衍生物、甲基纤维素,丙烯酸甲基纤维素,乙基纤维素等高分子聚合物。上述水溶性高分子的分子量并不特别限定,较佳而言,水溶性高分子选自淀粉、部份皂化、完全皂化的聚乙烯醇或其混合物。吸水性树脂含此等添加水溶性高分子的重量百分比介于为0%至20%之间,较佳介于0%至10%之间,更佳介于0%至5%之间。当水溶性高分子的添加量超过20%时,会影响聚合物的物性,使物性变差。
在进行自由基聚合反应前,可于单体溶液中添加自由基聚合反应交联剂。借由添加自由基聚合反应交联剂,可以使得反应后的吸水性树脂具有适当交联度,而使吸水性树脂胶体有适当的加工性。自由基聚合反应交联剂可单独使用或两种以上混合使用。自由基聚合反应交联剂的重量百分比可介于0.001%至5%之间(以反应物总固形份为基准),较佳介于0.01%至3%之间。当自由基聚合反应交联剂的添加量在重量百分比0.001%以下时,会导致聚合后的水凝胶体太软且有黏性,因而不利于机械加工。当自由基聚合反应交联剂的添加量在重量百分比5%以上时,则会导致吸水性太低,降低了吸水性树脂的性能。
上述自由基聚合反应交联剂可选用具有两个或两个以上不饱和双键的化合物,例如:N,N’-双(2-丙烯基)胺、N,N’-次甲基双丙烯酰胺、N,N’-次甲基双甲基丙烯酰胺、丙烯酸丙烯酯、乙二醇二丙烯酸酯、聚乙二醇二丙烯酸酯、乙二醇二甲基丙烯酸酯、聚乙二醇二甲基丙烯酸酯、甘油三丙烯酸酯、甘油三甲基丙烯酸酯、甘油附加环氧乙烷的三丙烯酸酯或三甲基丙烯酸酯、三甲醇丙烷附加环氧乙烷的三丙烯酸酯或三甲基丙烯酸酯、三甲醇丙烷三甲基丙烯酸酯、三甲醇丙烷三丙烯酸酯、N,N,N-三(2-丙烯基)胺、二丙烯酸乙二醇酯、三丙烯酸聚氧乙烯甘油酯、三丙烯酸二乙基聚氧乙烯甘油酯、二丙烯三甘醇酯等,也可选用具有两个或两个以上环氧基的化合物,例如:山梨醇聚缩水甘油醚、聚丙三醇聚缩水甘油醚、乙二醇二缩水甘油醚、二乙二醇二缩水甘油醚、聚乙二醇二缩水甘油醚、双丙三醇聚缩水甘油醚等,但不限于此。
为了控制成品的酸碱值(pH值),使其呈中性或微酸性,含酸基单体的羧酸基应该被部分中和。用于调整pH值的中和剂可以为周期表中碱金族或碱土族的氢氧化物或是碳酸化合物,例如:氢氧化钠、氢氧化钾、碳酸钠、碳酸钾、碳酸氢钠、碳酸氢钾、氨类化合物或其混合物。中和剂可单独使用一种或多种混合使用。借由添加中和剂,含酸基单体的羧酸基会部分被中和成钠盐、钾盐或铵盐。较佳来说,摩尔百分比为45mol%至85mol%的含酸基单体会被中和,更佳为50mol%至75mol%。当含酸基单体被中和的浓度摩尔百分比为45mol%以下时,会导致成品的pH值偏低,而当含酸基单体被中和浓度摩尔百分比为85mol%以上时,成品的pH值会偏高。当成品pH值非呈中性或微酸性时,其不适合与人体直接接触,也较不安全。
对于上述的自由基聚合反应,单体溶液中通常应加入聚合引发剂,借由聚合引发剂产生自由基,以使自由基聚合反应开始进行。聚合引发剂的适当用量为重量百分比介于0.001%至10%之间(以中和丙烯酸盐重量为基准),更佳则在重量百分比0.1%至5%之间。当其重量百分比为0.001%以下时,会导致反应太慢,不利经济效益。当其重量百分比为10%以上时,则反应太快,致使反应热不易控制,且容易聚合过度而形成凝胶状固体。
上述聚合引发剂可以是热分解型起始剂、氧化还原型起始剂或两者的混合。对于热分解型起始剂而言,其可以是过氧化物或偶氮化合物。举例来说,过氧化物可例如是:过氧化氢、二-第三丁基过氧化物、过氧化酰胺或过硫酸盐(铵盐、碱金属盐)等。偶氮化合物可例如是:2.2’-偶氮基双(2-脒基丙烷)二盐酸盐、2.2’-偶氮基双(N,N-二伸甲基异丁脒)二盐酸盐。此外,对于氧化还原型起始剂而言,其可以是还原剂,例如:酸性亚硫酸盐、硫代硫酸盐、抗坏血酸或亚铁盐。此外,聚合引发剂也可以同时包括氧化还原型起始剂和热分解型起始剂。对于聚合引发剂也同时包括氧化还原型起始剂和热分解型起始剂的情形,在自由基聚合反应的初始阶段,氧化还原起始剂会先进行反应,而产生自由基,当自由基转移至单体上时即会引发聚合反应的进行。由于聚合反应进行时会释放出大量的热量而使温度升高,当温度到达热分解型起始剂的分解温度时,又会引发第二段热分解型起始剂的分解,而使整个聚合反应更臻于完全。
上述自由基聚合反应可于传统批次反应容器中或于输送带式反应器上进行反应。反应所得的凝胶体,先利用绞碎机切成直径20mm以下小凝胶体,更佳是小于直径10mm。
在制造得到小凝胶体之后,后续可再进行筛选。在筛选程序中,以筛选直径2.00mm以下的凝胶体为宜,更佳为介于0.05mm至1.50mm间的凝胶体。对于粒径大于2.00mm的凝胶体则重新送回反应器中进行再次切碎。需注意的是,若对粒径0.03mm以下的凝胶体进行烘干、粉碎处理,容易造成成品有较高的细粉量,若对粒径2.00mm以上的凝胶体进行烘干时,容易因为热传导效果不佳,导致成品残存单体偏高,而导致其他物性表现不佳的缺点。依据本发明的实施例,当丙烯酸盐凝胶体的颗粒大小分布越窄时,不仅可使烘干后的凝胶体具有最佳的物性表现,而且有利于控制烘干的时间及温度。
在经过上述的筛选程序后,再进行烘干程序。烘干温度较佳介于100℃至180℃。若烘干温度在100℃以下,则会导致烘干时间太久,不具经济效益,若烘干温度在180℃以上,则烘干会使交联剂提早进行交联反应,使得后续的干燥过程中,因交联度过高而无法有效的去除残存单体,无法达到降低残存单体的效果。
在上述干燥程序之后,再进行粉碎、筛选固定粒径。筛选固定粒径较佳介于0.06mm至1.00mm之间,更佳介于0.10mm至0.850mm之间。当粒径在0.06mm以下时,细微颗粒会使成品的粉尘提高,当粒径大于1.00mm以上时,会使成品的吸水速率变慢。依据本发明的实施例,丙烯酸盐聚合物的颗粒大小分布越窄越好。
经过上述程序所制得的吸水性树脂为不溶解化的亲水性聚合体,树脂内部具有均匀性的架桥结构。为了进一步改善吸水性树脂的特性,例如:提高吸收速率、提高胶体强度、提高抗结块性、增加液体渗透性等特性,会进一步在树脂的表面涂覆具有能与酸基反应的多官能基交联剂,以在吸水性树脂的表面产生交联、架桥。以下就表面交联剂及表面交联处理加以叙述。
具体来说,在筛选固定粒径之后,可再进行表面交联剂涂覆处理,致使吸水性树脂的表面进一步产生交联。因此,可以让吸水性树脂的表层相对于其核心具有更高的交联度。此表层交联度较高且核心交联度较低的吸水性树脂又被称作是具有‘壳-核(core-shell)结构’的吸水性树脂。
上述表面交联剂的添加方式会依据表面交联剂的种类而有所不同。举例来说,可分成:表面交联剂直接添加、调成表面交联剂水溶液添加,或调成表面交联剂亲水性有机溶剂水溶液后再添加,其中亲水性有机溶剂可以选自甲醇、乙醇、丙醇、异丁醇、丙酮、甲醚、乙醚等,没有特殊限制,可形成溶液即可,更佳选自甲醇或乙醇(参照美国专利US6849665)。交联剂的适当添加剂量在重量百分比0.001%至10%之间(以反应物总固形份为基准),更佳在0.005%至5%之间。当交联剂添加剂量在重量百分比0.001%以下时无法显出效果,而当交联剂添加剂量在重量百分比10%以上时,吸水性太低,造成树脂性能降低。
根据本发明的一实施例,上述的交联剂可选用可同时进行表面处理及反应的交联剂,例如:多元醇、多元胺、具有两个或两个以上环氧基的化合物、碳酸亚烃酯或其混合物。具体来说,多元醇可以选自丙三醇、乙二醇、二乙二醇、三乙二醇、聚乙二醇或丙二醇等,但不限于此;多元胺可以选自乙二胺、二乙二胺或三乙二胺,但不限于此;具有两个或两个以上环氧基的化合物可以选自山梨醇聚缩水甘油醚、聚丙三醇聚缩水甘油醚、乙二醇二缩水甘油醚、二乙二醇二缩水甘油醚、聚乙二醇二缩水甘油醚或双丙三醇聚缩水甘油醚等,但不限于此;碳酸亚烃酯可以选自乙二醇碳酸酯、4-甲基-1,3-二氧杂环戊烷-2-酮、4,5-二甲基-1,3-二氧杂环戊烷-2-酮、4,4-二甲基-1,3-二氧杂环戊烷-2-酮、4-乙基-1,3-二氧杂环戊烷-2-酮、1,3-二氧杂环己烷-2-酮或4,6-二甲基-1,3-二氧杂环己烷-2-酮或1,3-二氧杂环庚烷-2-酮等,但不限于此。交联剂的用法可单独使用或两种以上混合使用。
现有专利文献已公开多种表面交联处理的程序,例如:将吸水性树脂与交联剂分散于有机溶剂中,以进行表面交联处理(JP-A-56-131608、JP-A-57-44627、JP-A-58-42602、JP-A58-117222);使用无机粉,直接将交联剂与交联剂溶液混入吸水性树脂,以进行表面交联处理(JP-A60-163956、JP-A-60-255814);添加交联剂后以蒸气处理(JP-A-1-113406);使用有机溶剂、水及多元醇进行表面处理(JP-A-1-292004、US6346569);使用有机溶液、水、醚(ether)化合物(JP-A-2-153903)等,现行专利文献所公开的表面交联处理的方法虽能提高吸收速率以及提高压力下吸水倍率,然而其也同时造成保持力下降过多的不良后果,降低了实际应用的性能。相较之下,本发明实施例所施行的表面交联处理的方法则不会存在上述缺失。
在施行上述表面交联处理之后,会进一步将表面交联处理后的高吸水性树脂与具有弱酸性含硅化合物的水溶液进行表面处理,以可得到同时具有抑菌及除臭能力,而且不会降低吸水特性的吸水性树脂。
根据本发明的一实施例,弱酸性含硅化合物水溶液适当添加剂量在重量百分比0.001%至20%之间(以反应物总固形份为基准),更适当的用量在0.005%至10%之间,含硅化合物水溶液添加剂量在重量百分比0.001%以下时无法显出效果,含硅化合物水溶液添加剂量在重量百分比20%以上时,吸水能力降低(如:压力下吸水倍率),降低树脂性能。
为了使弱酸性含硅化合物可均匀分布于吸水性树脂的表面,根据本发明的一实施例,可采用足以产生够大混合力的混合装置,使混合能够充分均匀。上述的混合装置可以是V-型混合器、柱式混合器、高速搅拌混合器、螺旋式混合器、气流混合器、双臂捏合机、双臂锥形混合器、螺条混合器、密壁式混合器、粉碎捏合机、旋转混合器或螺杆挤出机,但不限于此。
上述弱酸性含硅化合物的水溶液可经由下列两种方式获得:
(1)自行配制弱酸性含硅化合物的水溶液
利用硅藻土、软土、黏土、滑石粉、沸石、高岭土、膨土、活性白土、水滑石、凹凸棒或萤石等无机盐粉末与水混合所产生的水溶液;无机盐粉末的用法可单独使用或合并两种以上混合使用。其中,无机盐粉末中较佳含有氧化铝与二氧化硅,例如是含铝的硅酸盐。其中,氧化铝具有吸附异味能力,而二氧化硅则具有较多的负电量(-200uC/g),因而可以使无机盐粉末整体带负电。具体来说,硅化合物盐粉末能以离子键的形式对包覆病毒外部的蛋白质层产生键结,并对蛋白质产生破坏,当病毒的蛋白质结构一但遭到破坏,便无法继续生存及复制,因此可达到抑制其生长的效果。
需注意的是,为了达到吸附异味和抑菌的能力,上述无机粉末中氧化铝与二氧化硅的重量比较佳介于0.5-0.95之间,更佳介于0.7-0.95之间。对于氧化铝含量过低的情况,因此会导致异味吸附能力效果不佳。此外,对于氧化铝含量太高(即二氧化硅含量太低)的情况,由于二氧化硅的带电量(-200uC/g)远高于氧化铝的带电量(100uC/g),则会导致弱酸性含硅化合物的带负电荷量降低,导致细菌捕捉下降,进而无法抑制其生长。
无机盐粉末的粒径小于50um、较佳小于10um、更佳小于5um。弱酸性含硅化合物使用时需调配成水溶液,使其pH值介于4-6.5之间。由于水溶液为弱酸性,因此能与尿液中的氨类化合物物质进行酸碱中和反应,进一步提升降低异味效果。调整pH值所使用的酸性化合物可为碳酸氢钠、硫酸氢钠、乙酸、酒石酸、柠檬酸或硼酸等。无机盐粉末在水溶液中的含量介于重量百分比0.1%至30%之间(以反应物总固体量为基准),更适当的用量在0.5%至20%之间,无机盐粉末在水溶液浓度在重量百分比0.1%以下时无法显出效果,在重量百分比30%以上时,无机盐粉末无法有效的分散在水中。
为了使无机盐粉末和水能充分混合均匀,混合过程中所利用的混合装置须具能够产生大的混合力,例如:IKA MHD-200型混合机、IKA T25型混合机、IKA magic Lab DR型混合机、FMCE-1000型混合机或Ashizawa PSI-MIX等固液混合机。
(2)购买市售的无机盐水溶液
市售弱酸性含硅化合物的无机盐水溶液可例如是:LMC-581(珑茂公司制)、SH-2778(绅鸿公司制)、MY-972(铭烨公司制)等。
根据上述实施例,利用弱酸性含硅化合物水溶液喷洒于吸水性树脂的表面,即可制造同时具有抑菌及除臭能力的吸水性树脂,而且不会降低吸水性树脂的吸水特性。具体来说,吸水性树脂中的弱酸性含硅化合物可以和尿液中的酸性物质进行酸碱中和反应,借此达到降低异味发生。此外,借由弱酸性硅化合物具有高电荷性的特性,其可形成强大的静电吸附力,以捕捉细菌并抑制其生长。此外,借由弱酸性硅化合物的大表面积,其可吸附尿液中的硫化物或胺基化合物,而达到抑制异味的发生。另一方面,生产此吸水树脂时不会有无机盐粉末泄漏于生产设备,甚至于悬浮于厂房空气,进而伤害人员呼吸道的风险。用来制备合于上述的水溶性不饱和单体的步骤并无特殊的限制,只要经由本发明的方法制造所得的吸水性树脂,将能适用于各种型式的卫生用品、农业用及食品保鲜用的吸水剂。
上述实施例所公开的吸水性树脂适用于各种型式的卫生用品、农业用及食品保鲜用的吸水剂,其特别适合纸尿裤中的吸收体,尤其是低浓度纸浆尿裤(Fluffless,同时使用大量的吸水性树脂)及成人纸尿裤。
对于做为纸尿裤吸收体的吸水性树脂,不仅需具备一定吸收液体量的能力,也即保持力(Centrifuge Retention Capacity,CRC),更需具备较高的压力下通液性指数(PUL,Permeability Under Load)值。具体而言,对于同时具备高压力下吸水倍率(AbsorptionAgainst Pressure,AAP)及高压力下液体通透性的吸水性树脂,即便当液体进入已吸收液体的吸收体时,因其具备高压力下液体通透性,所以仍可以使液体容易通过已经吸收液体的吸水性树脂,从而扩散至其他未吸收液体的吸水性树脂,进而降低吸收体的回渗量(Rewet),并提升了纸尿裤的干爽性。在4.9kPa的压力下,对于0.9%的氯化钠水溶液而言,PUL值较佳高于30%以上,更佳高于40%以上。
根据本发明的实施例,吸收体为将吸水性树脂及亲水性纤维压制成型,而为片状的结构。吸收体下方可设置不透液性的高分子膜,例如PE膜,而透液性的不织布则设置于吸收体上方,以作为表层。此外,也可将吸水性树脂固定于纸浆纤维材料(Airlaid)和/或不织布上,纸浆纤维为粉碎的木浆、交联纤维素纤维、棉、羊毛或醋酸乙烯纤维等,但不限定于此。吸收体中吸水性树脂含量(芯体浓度)可介于重量百分比20%至100%之间,较佳介于重量百分比40%至100%之间,更佳介于50%至100%之间。根据本发明的实施例,吸收体的基重(单位面积重量)介于0.01-0.30g/cm2之间,吸收体厚度为30mm以下。
借由使用上述实施例所制备的吸水性树脂作为纸尿裤中的吸收体,其可以抑菌、除臭及维持吸水性树脂的吸水特性等,因此有效地解决了现有纸尿裤的问题。
为了使本发明所属技术领域的普通技术人员能够据以实施本发明,下文将进一步详细描述本发明吸水树脂和吸收体的物性分析方法以及具体制备方法。需注意的是,以下实施例仅为例示性,不应用以限制解释本发明。因此,在不逾越本发明范畴的情况下,可适当地改变各实施例中所采用的材料、材料的用量及比率以及处理流程等。需注意的是,在下文的物性分析方法,除非另有说明,均在于室温23±2℃及相对空气湿度45±10%下进行,且吸水性树脂分析前应进行充分混合。
以下先就吸水树脂和吸收体的物性分析方法加以介绍,各分析项目包括:吸水性树脂压力下液体的通透性、吸水性树脂压力下吸水倍率(AAP)、吸水性树脂压力下通液性指数(PUL)值、吸水性树脂保持力(CRC)、吸水性树脂残存单体(RAA:Residual Monomers)、吸水性树脂除臭测试、吸水性树脂抗菌试验、吸水性树脂恶臭去除试验、吸收体的回渗量评价、吸收体除臭测试、吸收体抗菌试验。
<吸水性树脂压力下液体的通透性>
依照EDANA(European Disposables And Nonwovens Association,欧洲不织布协会)规定ERT 443.1(5)的测试方法进行测试,测试在4.9kPa压力下吸水性树脂的液体通透性,较佳选用8(g/g)以上,更佳选用10(g/g)。
<吸水性树脂压力下吸水倍率>
依照EDANA规定ERT 442.2(5)的测试方法进行测试,测试吸水性树脂在4.9kPa的压力下,对于0.9%的氯化钠水溶液持续60分钟的压力下吸水倍率,较佳选用15(g/g)以上,更佳选用20-30(g/g)。
<吸水性树脂压力下通液性指数(PUL)值(单位:%)>
为压力下液体的通透性(PDAUP:Gravimeteric Determination of PermeabilityDependant Absorption Under Pressure)除以压力下吸水倍率(AAP:Absorption AgainstPressure)后再以百分比表示的结果。
<吸水性树脂保持力>
依照EDANA规定ERT 441.3(10)的测试方法进行测试。
<吸水性树脂残存单体>
依照EDANA规定ERT 410.3(10)的测试方法进行测试。
<吸水性树脂除臭测试>
收集成人尿液放置带盖的聚丙烯瓶中(尿液需排泄两小时内进行测试),加入2.0克吸水性树脂后,将聚丙烯瓶盖住,并将聚丙烯瓶置于37℃的环境下2小时。之后开盖,并在瓶口上方约3公分的位置,由10位成年人来嗅味道,并判定除臭效果。评判级别分成6等级,基准如下所示,并以所有人判级的平均值为最后评价结果,使用相同条件但不添加吸水性树脂的尿液味道为第5级。
0:无臭味
1:可稍为感觉到的臭味
2:可感觉到但可容许的臭味
3:感觉到的臭味
4:强臭味
5:浓烈臭味
<吸水性树脂抗菌试验>
依照AATCC(American Association of Textile Chemists and Colorists,美国纺织化学师与印染师协会)中的AATCC TM100-2012测试方法,分析对大肠杆菌的抗菌能力,若比对照组中大肠杆菌的繁殖量少,则视为具备抗菌能力。
<吸水性树脂恶臭去除试验(甲硫醇除去率测定试验)>
在1升的密闭容器中放入1.0克吸水性树脂和0.03%甲硫醇钠水溶液25毫升后,于室温下放置10分钟,之后利用气体检知管(GASTEC 4L及4HM)分析残留气体浓度。本试验中的去除率是以相对于空白试验的残留气体浓度的减少比率计算而得到。
<吸收体的回渗量(干爽性)评价>
放置4.8kPa(面积160平方厘米,重量7.8Kg)的重物于测试用吸收体,使得重物的重量均匀的作用于测试用吸收体上,之后于中心点分3次加入合成尿液(根据美国公开专利20040106745号所述的Jayco合成尿液)共180毫升(每次间隔30分钟),加完后,等待30分钟,之后除去测试用吸收体上方的重物,在测试用吸收体上放置预先测量总重量(W1(g))的滤纸(8厘米×20厘米)30张,再立即将4.8kPa的重物置于测试用吸收体上5分钟使上述滤纸吸收回渗的液体,然后测定30张滤纸的重量(W2(g))。吸收体的合成尿液回渗量(g)为W2-W1。回渗量越低,表示吸水树脂耐尿性越优良。
<吸收体除臭测试>
取10×10平方厘米的吸收体放于玻璃培养皿(内径120mm)中,收集成人尿液加入后,马上盖住密闭(尿液需排泄两小时内进行测试),并将玻璃培养皿置于37℃的环境下2小时,之后开盖,并在瓶口上方约3公分的位置,由10位成年人来嗅味道,并判定除臭效果。评判级别分成6等级,基准如下所示,并以所有人判级的平均值为最后评价结果,使用相同条件但不添加吸水性树脂的尿液味道为第5级。
0:无臭味
1:可稍为感觉到的臭味
2:可感觉到但可容许的臭味
3:感觉到的臭味
4:强臭味
5:浓烈臭味
<吸收体抗菌试验>
取10×10平方厘米的吸收体,使用AATCC100的方法,分析对大肠杆菌的抗菌能力,若比对照组中大肠杆菌的繁殖量少,则视为具备抗菌能力。
以下就弱酸性含硅化合物水溶液、吸水树脂、吸收体的制造方法加以介绍。
弱酸性含硅化合物水溶液调配方法
预备例1
将20克高岭土(购至珑茂公司/LM-812,粒径=2um,氧化铝与二氧化硅重量比为0.86)缓慢加入380克pH=5.0碳酸氢钠水溶液中(以0.25克/分钟条件进行添加,历时1.5小时),同时利用IKA T25型混合机进行混合(转速16000rpm),并保持系统的温度在5℃至15℃范围内,添加完毕后,再保持相同条件下,搅拌5分钟,即得弱酸性含硅化合物水溶液(1)。
吸水性树脂的制造方法
制造例1
(1)取48%氢氧化钠水溶液437.5g缓慢加入540g丙烯酸及583.2g的水的2000c.c圆锥瓶中,氢氧化钠/丙烯酸的滴加比率在0.85至0.95范围内,滴加时间为2小时,并保持瓶内中和反应系统的温度在15℃至40℃范围内。此时得单体在水溶液中的重量百分比浓度为42%,其中70mol%(摩尔比)的丙烯酸部分中和成为丙烯酸钠。
(2)再加入1.1g的N,N’-次甲基双丙烯酰胺于水溶性不饱和单体溶液,温度维持于20℃左右。
(3)加入0.3g双氧水,3.6g亚硫酸氢钠及3.6g过硫酸铵起始剂反应。
(4)将反应后生成的凝胶体利用切式粉碎机切碎,并筛选出粒径大小为2mm直径以下的凝胶体。
(5)再以130℃温度干燥2小时,之后利用0.1mm~0.85mm固定粒径筛网筛选,得粉状吸水性树脂,其测定保持力为40.5g/g。
(6)秤取粉状吸水性树脂200g,加入乙二醇、1,4-丁二醇(台湾塑料公司制造)及甲醇的1/1/0.5混合水溶液5g(乙二醇、1,4-丁二醇及甲醇的重量比例为1:1:0.5),以150℃温度加热处理1小时,冷却后,即得吸水性树脂。其测定保持力为32.3g/g,压力下吸水倍率23.7g/g,压力下液体的通透性10.4g/g,PUL=43.9%,残存单体352ppm。
制造例2
(1)取48%氢氧化钠水溶液437.5g缓慢加入540g丙烯酸及583.2g的水的2000c.c.圆锥瓶中,氢氧化钠/丙烯酸的滴加比率在0.85至0.95范围内,滴加时间为2小时,并保持瓶内中和反应系统的温度在15℃至40℃范围内;此时单体在水溶液中的重量百分比浓度为42%,其中70mol%(摩尔比)的丙烯酸会被部分中和成为丙烯酸钠。
(2)再加入1.5g的聚乙二醇二丙烯酸酯(分子量523)于水溶性不饱和单体溶液,温度维持于20℃左右。
(3)加入0.3g双氧水,3.6g亚硫酸氢钠及3.6g过硫酸铵起始剂,进行聚合反应。
(4)将反应后生成的凝胶体利用切式粉碎机切碎,并筛选出粒径大小为2mm直径以下的凝胶体。
(5)再以130℃温度干燥2小时;利用0.1mm~0.85mm固定粒径筛网筛选,得粉状吸水性树脂,其测定保持力为41.3g/g。
(6)秤取粉状吸水性树脂200g,加入乙二醇、1,4-丁二醇及甲醇的混合水溶液5g(乙二醇、1,4-丁二醇及甲醇的重量比例为1:1:0.5),以150℃温度加热处理1小时,冷却后,即得吸水性树脂。其测定保持力为33.1g/g,压力下吸水倍率24.6g/g,压力下液体的通透性12.2g/g,PUL=49.6%,残存单体412ppm。
以弱酸性含硅化合物水溶液对吸水性树脂进行表面处理
实施例1
秤取制造例1所制得吸水性树脂100g,加入LMC-581(珑茂公司制)0.7g,以V-型混合器混合处理5分钟,即得高性能吸水性树脂。其测定保持力为32.3g/g,压力下吸水倍率23.5g/g,压力下液体的通透性10.8g/g,PUL=46.0%,残存单体330ppm。
实施例2
重复实施例1,但LMC-581的添加量提高至1.5g。其余同实施例一,得高性能吸水性树脂,测定保持力为32.5g/g,压力下吸水倍率23.3g/g,压力下液体的通透性10.0g/g,PUL=42.9%,残存单体361ppm。
实施例3
重复实施例1,但使用MY-972(铭烨公司制)替代LMC-518。其余同实施例1,得高性能吸水性树脂,测定保持力为32.5g/g,压力下吸水倍率23.1g/g,压力下液体的通透性10.4g/g,PUL=45.0%,残存单体369ppm。
实施例4
重复实施例1,但以预备例1的稀释的弱酸性含硅化合物水溶液(1)(与水的比率为1:20,水溶液pH为5.1)替代LMC-518。其余同实施例1,可得高性能吸水性树脂,测定保持力为32.2g/g,压力下吸水倍率22.9g/g,压力下液体的通透性9.5g/g,PUL=41.5%,残存单体345ppm。
实施例5
重复实施例4,但稀释的弱酸性含硅化合物水溶液(1)添加量提高至2.0g。其余同实施例4,得高性能吸水性树脂,测定保持力为32.1g/g,压力下吸水倍率22.5g/g,压力下液体的通透性9.8g/g,PUL=43.6%,残存单体371ppm。
实施例6
秤取制造例2所制得吸水性树脂100g,加入0.7g的LMC-581,以V-型混合器混合处理5分钟,即得高性能吸水性树脂。其测定保持力为32.9g/g,压力下吸水倍率24.7g/g,压力下液体的通透性12.4g/g,PUL=50.2%,残存单体411ppm。
实施例7
重复实施例4,但使用制造例2所制得吸水性树脂。其余同实施例4,得高性能吸水性树脂,测定保持力为32.7g/g,压力下吸水倍率23.7g/g,压力下液体的通透性11.6g/g,PUL=48.9%,残存单体405ppm。
比较例1
重复实施例1,但是取1.5g的二氧化硅水溶液(Wacker公司制,型号HDKD1512B)替代LMC-518,其余同实施例1,得高性能吸水性树脂,测定保持力为32.5g/g,压力下吸水倍率21.4g/g,压力下液体的通透性6.0g/g,PUL=28.0%,残存单体374ppm。
比较例2
重复比较例1,但以预备例1稀释后的弱酸性含硅化合物水溶液(高岭土(粒径=2um),与水的比率为1:20,水溶液pH为7.1)替代二氧化硅水溶液,其余同比较例1,得高性能吸水性树脂,测定保持力为32.5g/g,压力下吸水倍率22.7g/g,压力下液体的通透性6.5g/g,PUL=22.7%,残存单体381ppm。
比较例3
重复实施例4,但使用凹凸棒土(珑茂公司,粒径=5um,氧化铝与二氧化硅重量比为0.12)替代弱酸性含硅化合物水溶液(1),以制得吸水性树脂,得高性能吸水性树脂,测定保持力为32.3g/g,压力下吸水倍率21.1g/g,压力下液体的通透性5.2g/g,PUL=24.6%,残存单体435ppm。
比较例4
制造例1即为比较例4。
比较例5
制造例2即为比较例5。
表1为除臭测试及抗菌试验结果。
表1
吸收体的制备方法
制备例1
取制造例1所得的吸水性树脂,使用吸收体成形机,将10.0克吸水性树脂与10.0克粉碎木浆进行混合成形,成形网目为400目(38um)金属网,吸收体面积为160平方厘米(8厘米×20厘米)。将成形后的吸收体放置于PE膜上方,再放置不织布后,将吸收体用18.39kPa(面积160平方厘米,重量30Kg)的压力压5分钟后,四周用白胶黏住,即得测试用吸收体(1)。吸收体(1)基重为0.07g/cm2,厚度为17mm。
制备例2
取实施例2所得的吸水性树脂,以类似制备例1中所述吸收体的制造方法制得吸收体(2),基重为0.07g/cm2,厚度为16mm。
制备例3
取实施例3所得的吸水性树脂,以类似制备例1中所述吸收体的制造方法制得吸收体(3),基重为0.07g/cm2,厚度为16mm。
制备例4
取实施例4所得的吸水性树脂,以类似制备例1中所述吸收体的制造方法制得吸收体(4),基重为0.08g/cm2,厚度为15mm。
制备例5
取实施例5所得的吸水性树脂,以类似制备例1中所述吸收体的制造方法制得吸收体(5),基重为0.07g/cm2,厚度为15mm。
制备例6
取实施例7所得的吸水性树脂,以类似制备例1中所述吸收体的制造方法制得吸收体(6),基重为0.08g/cm2,厚度为14mm。
对照例1
重复制备例1,但取比较例1得的吸水性树脂,其余同制备例1,制得吸收体(7),基重为0.07g/cm2,厚度为16mm。
对照例2
重复制备例1,但取比较例2得的吸水性树脂,其余同制备例1,制得吸收体(8),基重为0.08g/cm2,厚度为15mm。
对照例3
重复制备例1,但取比较例3得的吸水性树脂,其余同制备例1,制得吸收体(9),基重为0.07g/cm2,厚度为16mm。
表2为吸收体性能评价除臭测试及抗菌试验结果。
表2
除臭测试 | 抗菌试验 | 合成尿液回渗量 | |
制备例1 | 第3级 | 有 | 2.1g |
制备例2 | 第2级 | 有 | 2.8g |
制备例3 | 第3级 | 有 | 2.5g |
制备例4 | 第2级 | 有 | 3.2g |
制备例5 | 第3级 | 有 | 2.7g |
制备例6 | 第3级 | 有 | 2.9g |
对照例1 | 第5级 | 无 | 7.3g |
对照例2 | 第4级 | 无 | 8.5g |
对照例3 | 第5级 | 无 | 8.9g |
须注意的是,比较表1和表2,由于吸收体中仅吸水性树脂具备除臭及抗菌能力,而木浆及不织布并无此特性,所以表2中所示吸收体性能评价中的除臭测试效果会略低于表1中所示吸水性树脂的除臭测试效果。
当然,本发明还可有其它多种实施例,在不背离本发明精神及其实质的情况下,熟悉本领域的技术人员可根据本发明作出各种相应的改变和变形,但这些相应的改变和变形都应属于本发明权利要求的保护范围。
Claims (12)
1.一种吸水性树脂,其特征在于,该吸水性树脂包括:
多个树脂颗粒,各该树脂颗粒具有内部交联结构;
一表面交联剂,该表面交联剂键结于各该树脂颗粒的表面;以及
多个含硅无机盐类颗粒,该多个含硅无机盐类颗粒覆盖住各该树脂颗粒的表面。
2.根据权利要求1所述的吸水性树脂,其特征在于,各该树脂颗粒借由具有不饱和双键的亲水性单体聚合而成。
3.根据权利要求1所述的吸水性树脂,其特征在于,各该含硅无机盐类颗粒的组成包括氧化铝及二氧化硅。
4.根据权利要求3所述的吸水性树脂,其特征在于,各该含硅无机盐类颗粒中氧化铝及二氧化硅间的重量比介于0.7至0.95。
5.根据权利要求1所述的吸水性树脂,其特征在于,各该含硅无机盐类颗粒的粒径介于1-10um。
6.根据权利要求1所述的吸水性树脂,其特征在于,各该含硅无机盐类颗粒的组成为高岭土。
7.一种吸水性树脂的制造方法,其特征在于,包括:
(a)提供一酸基单体水溶液,并进行一自由基聚合反应,以制得具有内部交联结构的吸水性树脂;
(b)切碎该吸水性树脂,以获得多个吸水性树脂颗粒;
(c)添加一表面交联剂于各该吸水性树脂颗粒的表面,并进行热处理;以及
(d)将一含有多个含硅无机盐类颗粒的水溶液涂覆于各该吸水性树脂颗粒的表面。
8.根据权利要求7所述的吸水性树脂的制造方法,其特征在于,该含有多个含硅无机盐类颗粒的水溶液的pH值介于4-6.5间。
9.根据权利要求7所述的吸水性树脂的制造方法,其特征在于,该含有多个含硅无机盐类颗粒的水溶液和该多个吸水性树脂颗粒间的重量百分比介于0.5%至20%。
10.根据权利要求7所述的吸水性树脂的制造方法,其特征在于,各该含硅无机盐类颗粒中氧化铝及二氧化硅间的重量比介于0.7至0.95。
11.根据权利要求7所述的吸水性树脂的制造方法,其特征在于,各该含硅无机盐类颗粒的粒径介于1-10um。
12.根据权利要求7所述的吸水性树脂的制造方法,其特征在于,各该含硅无机盐类颗粒的组成为高岭土。
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CN112852433A (zh) * | 2020-12-30 | 2021-05-28 | 北京化工大学 | 一种污染场地异味控制剂及制备方法 |
CN116531176A (zh) * | 2023-05-18 | 2023-08-04 | 佛山市中柔日用品有限公司 | 一种吸收制品及其制备方法 |
CN116531176B (zh) * | 2023-05-18 | 2023-10-24 | 佛山市中柔日用品有限公司 | 一种吸收制品及其制备方法 |
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US20180282507A1 (en) | 2018-10-04 |
TW201837107A (zh) | 2018-10-16 |
EP3381970A1 (en) | 2018-10-03 |
CN108659434B (zh) | 2020-10-20 |
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