CN1197462A - 水和含水液体的吸收剂及其生产方法和应用 - Google Patents
水和含水液体的吸收剂及其生产方法和应用 Download PDFInfo
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- CN1197462A CN1197462A CN96197170A CN96197170A CN1197462A CN 1197462 A CN1197462 A CN 1197462A CN 96197170 A CN96197170 A CN 96197170A CN 96197170 A CN96197170 A CN 96197170A CN 1197462 A CN1197462 A CN 1197462A
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- 239000002689 soil Substances 0.000 claims abstract description 5
- 239000013543 active substance Substances 0.000 claims abstract description 4
- 210000001124 body fluid Anatomy 0.000 claims abstract description 3
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- 239000000126 substance Substances 0.000 claims description 64
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Abstract
本发明涉及一种粉状的,吸收水和含水液体的交联聚合物,该聚合物由聚合的、未饱和的、含酸基的并以中和到至少50mol%的盐而存在的单体组成,并可含有可与含酸基单体和水溶性聚合物共聚的其它单体,其中,聚合物由相对于含酸基单体组分的5—30mol%部分中和的酸性聚合单体组成。该聚合物是一种高保留值的、压力下有高的液体吸收值的吸收剂,它具有高膨胀压及低的可溶性组分。本发明还涉及所述聚合物的生产方法和涉及在吸收体液的卫生用品和绷带中,以及在电缆和光缆中作为组成的应用,还可用作地板改良材料,包装材料的组成,以及用于控制释放活性物质的贮存材料中。
Description
本发明涉及对水或含水液体具有高吸收容量的水不溶性的,水膨胀性的聚合物,该聚合物基于交联的,亲水性均聚物和共聚物,以及基于乙烯类未饱和的、含酸基的、可聚合单体的接枝聚合物。本发明进一步涉及这些聚合物的生产方法和应用。
能吸收大量含水液体,特别是体液例如尿的聚合物被称为高效吸收性聚合物。
如在US 4,286,082,DE 2706135,US 4,340,706,DE 3713601,和DE2840010中所描述的,吸收剂是由在水溶液中优选使用单乙烯类未饱和羧酸,例如丙烯酸及其碱式盐的自由基聚合,或按照反悬浮或乳液聚合法生产的。
具有不同吸收特性的聚合物可以通过选择单体组合物,交联剂,和聚合物凝胶的聚合条件和处理条件来生产。也有人提出了另外的可能性,即用接枝聚合物进行生产,例如根据DE 2612846,用化学改性淀粉,纤维素,和聚乙烯醇,和例如根据DE 4020780C1,通过对聚合物颗粒作二次表面交联或对聚合物凝胶或粉状树脂作后处理来生产。
为了这类聚合物在卫生和保健领域中的应用,生产的聚合物其中和度范围相对于聚合的含酸基单体单元来说应在50-80%之间,由此形成的水凝胶在使用时对皮肤具有中性效果。
中和度可用不同的方法调整,经常在聚合之前进行酸性单体的中和或部分中和。不过,含酸性聚合单体单元的水凝胶的中和或部分中和也是已知的。
根据EP 205674A1,在温度范围0-100℃,优选5-40℃下有利于生产完全酸性的聚合物,它将通过其后对水凝胶的部分中和来调整。该聚合物在改进凝胶强度和吸收容量,以及含少量的水溶性聚合物方面是突出的。
根据US 5145906和EP 530438B1,在温度范围为5-20℃,绝热,且无对单体中和的条件下生产出丙烯酸的聚合物凝胶并伴随水溶性含羟基聚合物;接着减小该聚合物凝胶粒度,并部分或完全地由水溶性碱中和,然后在二次交联剂的存在下加以粉碎,并进行热处理。
上述方法是不利的,因为如EP 467073A1所表明的该单体溶液的聚合反应发生得很慢,所以该反应只能以间歇方式间断地进行。增加引发剂的量和提高反应温度会影响所要求的聚合物性质。此外,粉碎全酸性聚合物凝胶是很困难的,且由扩散起支配作用的中和作用发生得很缓慢。在这种情况下,聚合物颗粒的表面区域保留了过量的碱,而仍有反应性的聚合的含酸基单体单元存在于凝胶的内部,不可用于其后表面区域的交联反应。
EP 467073A1描述了在控制聚合反应温度为20-70℃,特别是55-60℃下5小时内得到的聚合物。根据所述方法,然后将聚丙烯酸中和到72%度。接着将干燥和磨碎的聚合物进行其后的交联处理。不过,如果是在压力下吸收液体,则根据本方法得到的聚合物只具有限的液体吸收容量。另外,吸收液体之后,已知的聚合物具有显著的再湿润性,特别是当其用作卫生用品时是不利的。
因此,本发明的目的是提供具有改进吸收特性的聚合物,特别是在加压下它有改进的液体吸收性能和改进的再湿润性,还要提供以减少聚合时间和改进其后交联的生产方法。
本目的是以一种粉状的吸收水和含水液体的交联聚合物而实现的,该聚合物由下列组分形成:a)55-99.9重量%的至少一种聚合的、非饱和的、含酸基可聚合单体,它以中和到至少50mol%的盐存在,b)0-40重量%的一种聚合的、非饱和单体,它与a)的单体可共聚,c)0.01-5.0重量%的至少一种交联剂,和d)0-30重量%的一种水溶性聚合物,a)-d)的组分的总量为100%,该聚合物的特征在于,它是由相对于含酸基单体部分而言,部分中和到5-30mol%的酸性聚合物凝胶组成,且其具有
-对0.9%NaCl水溶液的保留量至少为25g/克聚合物,
-50g/cm2压力下,吸收液体至少为25g/克聚合物,
-20分钟后相对于1g聚合物的膨胀压力至少为700g,
-16小时后,最大可溶含量为3.5-10重量%,和
-最大再湿润为2.0g。
本目的进一步是由生产这种聚合物的方法实现的,其特征在于,制备一种水溶液,该水溶液相对于总溶液来说具有30重量%的最大单体含量;聚合之前,将非饱和的、可聚合的、含酸基单体用碱中和到5.0-30mol%,优选10-20mol%;在5-30℃,优选8-15℃的温度范围内,且在自由基条件下,用化学引发剂和/或UV-辐射引发,并持续绝热;聚合物凝胶经粗磨后,再经粉碎,且用碱中和,使聚合物含至少50mol%的经聚合的、中和的含酸基单体单元;聚合物凝胶干燥到水含量≤10重量%;在温度140-240℃范围内,将干燥和磨碎的聚合物与易与酸基反应的至少一种双-或多官能交联剂反应。
最令人意外的是,我们发现,如果使用一种,其中少量的含酸基单体已通过加碱中和的溶液,而不使用完全酸性的聚合物溶液来进行聚合反应,则得到了在常压或提高压力下具有高保留值和高吸收容量以及低可溶聚合物组分的聚合物。相对于含酸基单体而言,部分中和量的范围约为5-30mol%,优选为5-20mol%,更优选为5-10mol%。
根据本发明,用作可聚合的、非饱和的含酸基单体a)的是水溶性的单乙烯类未饱和的单-和二羧酸,例如丙烯酸,甲基丙烯酸,乙基丙烯酸,巴豆酸,山梨酸,马来酸,富马酸,衣康酸,以及乙烯基磺酸;丙烯酰胺-和/或甲基丙烯酰胺烷基磺酸,例如2-丙烯酰胺-2-甲基丙烷磺酸,2-异丁烯酰氧乙烷磺酸,4-苯乙烯磺酸,烯丙基磺酸,乙烯基甲苯磺酸,乙烯基膦酸,和苯乙烯膦酸。
丙烯酸是优选的水溶性非饱和羧酸。除丙烯酸外,聚合物中其它非饱和羧酸的比例可以高达重量50%。
用作单体b)的是水溶性单乙烯类未饱和单体,例如丙烯酰胺,甲基丙烯酰胺,N-烷基化(甲基)丙烯酰胺,N-羟甲基(甲基)丙烯酰胺,N-乙烯基酰胺,N-乙烯基甲酰胺,N-乙烯基乙酰胺,和N-乙烯基-N-甲基乙酰胺,N-乙烯基-N-甲基甲酰胺,乙烯基吡咯烷酮,以及羟烷基(甲基)丙烯酸酯,例如羟乙基丙烯酸酯和聚乙二醇单烯丙基醚的甲基丙烯酸酯,和聚乙二醇的烯丙基醚。
丙烯酸和甲基丙烯酸酯,例如丙烯酸乙酯和丙烯酸甲酯,醋酸乙烯酯和苯乙烯以其低水溶性,也可以有限量用作单体b)。这些难溶或微溶于水的单体的最大用量为全部单体总重量的10%。
所述的单体可用于生产按任何所需组合含至少两种单体的均聚物或共聚物。单体混合物可以另外含有相对于单体溶液组成重量的0-30%的水溶性聚合物d)。
其实例包括上述单体的水溶性均聚物和共聚物,例如聚丙烯酸,部分皂化的聚醋酸乙烯酯,聚乙烯醇,聚亚烷基二醇,淀粉,淀粉衍生物,接枝聚合淀粉,纤维素和纤维素衍生物,例如羧甲基纤维素,羟甲基纤维素,以及半乳甘露聚糖及其烷氧基化衍生物。
单体水溶液包括至少一种交联剂c),其重量含量相对于单体溶液组分a),b)和c)的全部重量的0.01-5.0%,优选0.1-2.0%。含至少两个乙烯未饱和双键,或一个乙烯类未饱和双键和一个对酸基有反应性的官能团,或几个对酸基有反应性的官能团的任何化合物都可用作交联剂。其例子包括:亚甲基双丙烯酰胺,多元醇的丙烯酸酯和异丁烯酸酯,例如丁二醇双丙烯酸酯,己二醇双异丁烯酸酯,聚乙二醇二丙烯酸酯,和三羟甲基丙烷三丙烯酸酯,和/或烷氧基化的上述多元醇的丙烯酸酯和异丁烯酸酯,例如烷氧基化的三羟甲基丙烷和烷氧基化的季戊四醇。此类型的交联剂是以商品名Sartomer和Craynor(Crayvalley KunstharzeGmbH,47918 Tonisvorst,Germany)而周知的,其中Sartomer415,Sartomer454,Sartomer494,Sartomer610,和Craynor435是特别适用的;此外,具有非饱和的一元羧酸和/或多元羧酸的多元醇和烷氧基化多元醇的二酯和聚酯,例如1,2-丙二醇,季戊四醇,甘油和聚甘油的(甲基)丙烯酸酯,以及具有非饱和的一元羧酸和/或一元羧酸的未饱和醇和乙氧基化非饱和醇的单酯,例如丙烯基丙烯酸酯和异丁烯酸酯,单丙烯基马来酸酯,丙烯基聚乙二醇醚丙烯酸酯和异丁烯酸酯,丙烯基衣康酸酯,丙烯基聚乙二醇醚衣康酸酯,和单丙烯基聚乙二醇醚马来酸酯;还有二丙烯基丙烯酰胺,二丙烯基酞酸酯,二丙烯基己二酸酯,三丙烯基柠檬酸酯,和三单丙烯基聚乙二醇柠檬酸醚;此外,二元醇和多元醇的丙烯基醚及其乙氧基化物,例如乙二醇,二乙二醇,聚乙二醇的二丙烯基醚,甘油,乙氧基化甘油,三羟甲基丙烷和乙氧基化的三羟甲基丙烷的三丙烯基醚,季戊四醇和乙氧基化的季戊四醇的四丙烯基醚,以及四丙烯基氧乙烷,和聚缩水甘油醚,例如乙二醇二缩水甘油醚和甘油缩水甘油醚。此外,胺和/或它们的盐以及具有至少两个乙烯类未饱和的烷基基团的氨化物,例如二或三丙烯基胺和四丙烯基氯化铵。
常用的引发剂被用于引发自由基聚合反应,例如,过氧和偶氮化合物,优选水溶性和/或游离过氧和偶氮化合物,例如叔丁基过氧化氢和2,2′-偶氮双(2-甲基二乙酮脒)二盐酸盐;以及由过氧化单硫酸钠和钾,过氧化二硫酸钠和钾,以及含亚硫酸钠和钾,甲脒亚磺酸钠和钾,与抗坏血酸的过氧化氢组成的氧化还原体系。
当使用氧化还原体系时,优选首先制备氧化剂,然后再加入还原剂。特别是在连续聚合的情况下,可采用紫外光和已知光敏剂的光催化来引发。
在加入单体溶液的其它组分之前,最好先将含酸基单体中和,并优选首先制备碱。合适的碱包括碱性氢氧化物,氨水,和脂肪族伯胺和仲胺,以及碱式碳酸盐和碱式碳酸氢盐。优选碱性氢氧化物,氢氧化钠和氢氧化钾,以及氨水和碳酸钠。
聚合反应之前,单体溶液被冷却到5-30℃,优选8-20℃。反应引发后,在无抑制效应的情况下发生聚合,即,在起始期和在聚合反应的进程中都无延迟;这是令人意外的,并与已知的方法不同。聚合反应以间断批量的方式或更有利地以连续的方式,例如在带式反应器内进行。
然后将形成的聚合物凝胶进行粗磨和用常用的研磨和/或切削工具进行粉碎。优选是经由具有多块末端破碎孔板的切削式挤出机进行粉碎,其孔直径范围为2-20mm,优选5-15mm,和更优选8-13mm。
粉碎的聚合物凝胶的后续中和是用上述碱进行部分中和,并还可使用氢氧化钠溶液和氢氧化钾溶液和/或氨水或碳酸钠,例如以Na2CO3.10H2O或以其水溶液。中和在简单混合设备,例如,转鼓或Drais混合器中进行,含碱水溶液被例如喷嘴或喷雾注射器引入。中和进行到至少50mol%,优选60-80mol%的含酸基聚合单体单元作为盐而存在。其后的中和也可以在凝胶粉碎期间完成,例如在挤出机中粒度减小期间完成。
由于单体碱液少部分的中和,聚合物凝胶对碱优选强碱液的亲合力,改善到这样的程度,以致用简单混合设备即足以在短时间内进行进一步的中和;极大程度地避免了聚合物凝胶的机械损害。
在温度范围为100-190℃,将聚合物凝胶干燥到含水为重量5-20%,优选≤10重量%。随后,将干燥产品研磨成聚合物粉体,粒度范围为20-3,000μm,优选150-850μm。聚合物的后续交联在干燥聚合物颗粒表面进行,采用至少一种双-或多官能交联剂与酸基,优选与羧基反应,该交联剂以含水的溶液形式优选使用。合适的二次交联剂包括多元醇,例如乙二醇,1,2-丙二醇,1,4-丁二醇,甘油,二-和聚甘油,季戊四醇,这些多元醇的乙氧基化物,以及它们与羧酸或碳酸的酯。有利地加入酯化作用催化剂,例如,对-甲苯磺酸或磷酸。进一步适合的交联剂包括多元醇和聚乙二醇的双-和聚缩水甘油醚。这种化合物是商业可得的,商品名为Denacol(Nagase(Europe)GmbH,Dusseldorf)。
后续交联在混合设备,例如Nara混合器中进行,其温度范围为150-250℃,优选为150-200℃。
根据本发明的生产方法提供的聚合物,突出表现在与通常的产品相比大大地改进了特性。在0.9%NaCl水溶液中,其保留量至少为25g/克聚合物,优选为至少33g/g聚合物。在50g/cm2压力负荷下,其液体吸收为至少25g/g聚合物,优选为至少27g/g聚合物。本发明的聚合物在吸收水或含水液体后会膨胀,该聚合物在膨胀的条件下,甚至在压力下对这些液体具有高的渗透性。因此,当液体连续地和重复地出现时,充分利用了该聚合物的吸收容量,获得了液体的良好分布。另外,只有很少量吸收的含水液体再释放出来,因此再湿润的最大值为2.0g,优选最大为1.0g。根据Stevens LFRA Texture分析仪的方法,它们吸收液体的容量进一步表征为非常高的膨胀压,至少为700g,优选至少为850g,和最优选至少为1,000g。根据本发明的聚合物,其可溶性聚合物含量部分低于10重量%,优选低于5重量%,和最优选低于3.5重量%。
根据本发明方法得到的吸收剂可以与另外的物质混合。这些物质包括如填料,例如白垩土,膨润土,或硅藻土,以及纤维性材料,例如***,粘胶丝,或纤维素纤维。色料,紫外吸收剂,抗氧剂,和农业化学品,例如肥料,除草剂,防霉剂,和杀虫剂也可用作组分。根据本发明的聚合物可以用于许多领域,优选为卫生产品,例如尿布,卫生巾,绷带,和失禁袋,该袋可用作快速和完全地吸收尿液,月经血,和伤口分泌物;另外,用作包装嵌入物的组成以吸收从食品中释放的液体,用作电缆填充材料的组成以防止水进入海底电缆,并在园艺和农业底质中,用作土壤调节剂,或作为活性物质控制释放的贮存材料。
本发明将在实施例中进行示范,其中使用了下列检测方法:
保留值(TB):
200g高效吸收剂称重后装入茶叶袋中,并浸入生理盐水(0.9重量%的NaCl)30分钟。之后,将茶叶袋的一角挂起10分钟以除去游离水分,然后在1,400rpm的离心机中离心。从结果重量中减去空白读数和初重,结果转换为1g(TBg/g)。
压力下的吸收值(AAP):
0.9g高效吸收剂均匀地分布在内径6mm的园筒中,园筒底部装有筛孔尺寸为35μm的筛网。在高效吸收剂上施加重为20g/cm3(AAP0.3psi)或50g/cm3(AAP0.7psi)的压力。将园筒称重,然后置于一陶瓷过滤板上,该陶瓷板被浸入生理盐水的相同水位外。1小时后,将园筒再称重。园筒重量之差与高吸收剂初重之商被取作吸收值[(W后-W前/初重)]。
再湿润:
根据EP0631768A1,p.19,1.39至p.20,1.4中的程度进行再湿润检测;不过,使用0.9%NaCl水溶液以代替人造尿。
膨胀压力(SP):
采用Stevens L.F.R.A.Texture分析仪测定膨胀压力SP,该分析仪来自C.Stevens & Son Ltd.,Laboratory division,St.Albans AL1 1 ExHertfordshire,England。粒度为20-50目的0.500g高效吸收剂称重后加入到直径2.7cm的测量筒内,并加入10毫升0.9%NaCl溶液。然后,测量筒用提升台提高,直到圆筒形测量仪的下缘和测量筒中样品的表面间的距离达到12mm。通过凝胶的膨胀,测量筒被推压至双通道负载感应室,装置上负载以克表示。
残留单体(RM):
用生理盐水萃取达到平衡态后,用气相色谱测定高效吸收剂中残留丙烯酸量。
可溶量(SC):
高效吸收剂中在16小时内可以被萃取的涉及羧酸的聚合物部分用EP专利中请0205674,pp.34-37中描述的方法进行测定;不过,使用了生理盐水,而不用人造尿。相对于干燥的,研磨的聚合物的数量是由重量%给出的。
将用下列实施例和比较数据对本发明作更详尽的说明:
实施例1:
将80g丙烯酸和0.24g乙氧基化(15mol氧化乙烯)三羟甲基丙烷三丙烯酸酯溶解在244g水中,并用4.4g 50%的氢氧化钠溶液预中和。用冰冷却到6-8℃并用氮吹洗到最大残余氧含量为0.3ppm后,加入0.033g2,2′-偶氮-双(2-甲基二乙酮脒)二盐酸盐,0.12g过硫酸钠,和0.023g过氧化氢(35%)。然后,用0.003g抗坏血酸开始聚合反应。
约5分钟的起始阶段后,温度不断上升,并在20分钟后达到最高温度72℃。再维持15分钟用于二次反应,然后将所得聚合物凝胶通过食品研磨机。然后在具有水平搅拌轴的转鼓中将粉碎的物质与57.8g 50%的氢氧化钠溶液混合(提高中和度到70%),在140-160℃下干燥至水含量<10%,并研磨至粒度>180至<850μm。在190℃下用乙二醇碳酸酯(0.5%绝对干燥,溶解在水/丙酮中)将得到的颗粒进行表面再交联。
实施例2:
将80g丙烯酸和0.2g乙氧基化(3mol氧化乙烯)三羟甲基丙烷三丙烯酸酯溶解在244g水中,并用8.9g 50%的氢氧化钠溶液预中和。用冰冷却到6-8℃并用氮吹洗到最大残余氧含量为0.3ppm后,加入0.033g 2,2′-偶氮-双(2-甲基二乙酮脒)二盐酸盐,0.12g过硫酸钠,和0.023g过氧化氢(35%)。然后,用0.003g抗坏血酸开始聚合反应。
约20分钟后,达到最高温度74℃。再维持15分钟用于二次反应,然后将所得聚合物凝胶通过食品研磨机。然后在具有水平搅拌轴的转鼓中将粉碎的物质与53.3g50%的氢氧化钠溶液混合(提高中和度到70%),在140-160℃下干燥至水含量<10%,并研磨至粒度>180至<850μm。在190℃下用乙二醇碳酸酯(0.5%绝对干燥溶解在水/丙酮中)将得到的颗粒进行表面再交联。
实施例3:
将80g丙烯酸和0.16g三羟甲基丙烷溶解在244g水中,并用8.9g50%的氢氧化钠溶液预中和。用冰冷却到6-8℃后,用氮吹洗到最大残余氧含量为0.3ppm,加入0.033g 2,2′-偶氮-双(2-甲基二乙酮脒)二盐酸盐,0.12g过硫酸钠,和0.023g过氧化氢(35%)。然后,用0.003g抗坏血酸开始聚合反应。
约20分钟后,达到最高温度74℃。再维持15分钟用于二次反应,然后将所得聚合物凝胶通过食品研磨机。然后在具有水平搅拌轴的转鼓中将粉碎的物质与53.3g50%的氢氧化钠溶液混合(提高中和度到70%),在140-160℃下干燥至水含量<10%,并研磨至粒度>180至<850μm。在190℃下用乙二醇碳酸酯(0.5%绝对干燥,溶解在水/丙酮中)将得到的颗粒进行表面再交联。
实施例4:
将80g丙烯酸和0.24g乙氧基化(15mol氧化乙烯)三羟甲基丙烷三丙烯酸酯溶解在244g水中,并用8.9g50%的氢氧化钠溶液预中和。用冰冷却到6-8℃并用氮吹洗到最大残余氧含量为0.3ppm后,加入0.033g 2,2′-偶氮-双(2-甲基二乙酮脒)二盐酸盐,0.12g过硫酸钠,和0.023g过氧化氢(35%)。用0.003g抗坏血酸开始聚合反应。
约20分钟后,达到最高温度74℃。再维持15分钟用于二次反应,然后将所得聚合物凝胶通过食品研磨机。然后在具有水平搅拌轴的转鼓中将粉碎的物质与53.3g 50%的氢氧化钠溶液混合(提高中和度到70%),在140-160℃下干燥至水含量<10%,并研磨至粒度>180至<850μm。在190℃下用乙二醇碳酸酯(0.5%绝对干燥,溶解在水/丙酮中)将得到的颗粒进行表面再交联。
实施例5:
将80g丙烯酸和1g聚乙烯(600)-乙二醇二丙烯酸酯连同1gMowiol5/88(Hoechst)溶解在240g水中,并用8.9g 50%的氢氧化钠溶液预中和。用冰冷却到6-8℃并用氮吹洗到最大残余氧含量为0.3ppm后,加入0.23g 2,2′-偶氮-双(2-甲基二乙酮脒)二盐酸盐和0.24g过氧化氢(35%)。然后,用0.02g抗坏血酸开始聚合反应。
约15分钟后,达到最高温度75℃。在15分钟的停止时间用于二次反应后,将所得聚合物凝胶通过食品研磨机。然后在具有水平搅拌轴的转鼓中将粉碎的物质与190.7g未焙烧过的固体碳酸钠混合(提高中和度到70%),在140-160℃下干燥至水含量<10%,并研磨至粒度>180至<850μm。在190℃下用乙二醇碳酸酯(0.5绝对干燥,溶解在水/丙酮中)将得到的颗粒进行表面再交联。
实施例6:
将80g丙烯酸和1g聚乙烯(400)-乙二醇二丙烯酸酯连同1gMowiol5/88(Hoechst)溶解在240g水中,并用26.7g 50%的氢氧化钠溶液预中和。用冰冷却到6-8℃并用氮吹洗到最大残余氧含量为0.3ppm后,加入0.23g 2,2′-偶氮-双(2-甲基二乙酮脒)二盐酸盐和0.24g过氧化氢(35%)。然后,用0.02g抗坏血酸开始聚合反应。约15分钟后,达到最高温度75℃。在20分钟的停止时间用于二次反应后,按实施例1所述进行进一步处理;将35.5g 50%氢氧化钠溶液用于其后的中和反应。
实施例7:
将80g丙烯酸和1g聚乙烯(400)-乙二醇二丙烯酸酯连同1gMowiol5/88(Hoechst)溶解在240g水中,并用4.5g 50%的氢氧化钠溶液预中和。用冰冷却到6-8℃并用氮吹洗到最大残余氧含量为0.3ppm后,加入0.23g 2,2′-偶氮-双(2-甲基二乙酮脒)二盐酸盐和0.24g过氧化氢(35%)。然后,用0.02g抗坏血酸开始聚合反应。约25分钟后,达到最高温度72℃。在20分钟的停止时间用于二次反应后,按实施例1所述进行进一步处理;将39.9g 50%氢氧化钠溶液用于其后的中和反应。
比较例1:
无预中和度的聚合反应试验:
将80g丙烯酸和0.24g乙氧基化(3mol氧化乙烯)三羟甲基丙烷三丙烯酸酯溶解在244g水中。用冰冷却到6-8℃并用氮吹洗到最大残余氧含量为0.3ppm后,加入0.033g 2,2′-偶氮-双(2-甲基二乙酮脒)二盐酸盐,0.12g过硫酸钠,和0.023g过氧化氢(35%)。然后,试图用0.003g抗坏血酸开始聚合反应(按实施例1)。聚合反应失败了,再加入0.02g抗坏血酸。约5分钟的停止时间后,聚合反应开始,并在约30分钟后达到最高温度64℃。再维持15分钟用于二次反应,然后将所得聚合物凝胶通过食品研磨机。然后在具有水平搅拌轴的转鼓中将粉碎的物质与62.2g氢氧化钠溶液混合(提高中和度到70%),在140-160℃下干燥至水含量<10%,并研磨至粒度>180至<850μm。在190℃下用乙二醇碳酸酯(0.5%绝对干燥,溶解在水/丙酮中)将得到的颗粒进行表面再交联。
表1
聚合物特性
TB(g/g) | AAP0.3(g/g) | AAP0.7(g/g) | SP20/120min.(g) | SC%重量 | Rewet(g) | |
实施例1 | 34 | 36 | 28 | 850/900 | 4.5 | 0.5 |
实施例2 | 35 | 36 | 29 | 880/920 | 5 | 1.0 |
实施例3 | 35 | 36 | 28 | 850/890 | 5 | 1.0 |
实施例4 | 35 | 36 | 29 | 860/920 | 5 | 1.0 |
实施例5 | 34 | 37 | 30 | 1040/940 | 4 | 0.2 |
实施例6 | 34 | 37 | 30 | 1120/925 | 5 | 1.0 |
实施例7 | 35 | 36 | 29 | 910/920 | 4 | 2.0 |
比较例1 | 32 | 34 | 25 | 820/850 | 4 | 2.5 |
Sanwet IM 4000* | 31 | 29 | 19 | 577/496 | 5.2 | 2.5 |
Sanwet IM 7000* | 35 | 29.5 | 16 | 609/522 | 5.4 | 2.9 |
Sanwet IM 7000* | 33 | 34 | 20 | 529/567 | 2.8 | 8.5 |
*来自Hoechst AG
表2×
具有不同中和度的酸性聚合物凝胶保留量(根据实施例2或比较例1,相对于丙烯酸的24%活性物质):
实施例 | 中和度(%) | TB(g/g) |
比较例1 | 0 | 2.04 |
2 | 5 | 2.25 |
2 | 10 | 2.80 |
2 | 20 | 4.96 |
2 | 30 | 8.90 |
表2中数据表明,以生理盐水保留值为基础,对丙烯酸聚合物凝胶在中和范围为0-30%的条件下,丙烯酸凝胶对含水液体的吸收容量有极大的提高。
Claims (18)
1.一种粉状、吸收水和含水液体的交联聚合物它包括
a)55-99.9重量%的至少一种聚合的、未饱和的、可聚合的含酸基单体,该单体作为一种中和到至少50mol%的盐而存在,
b)0-40重量%的聚合的未饱和单体,该单体与所述a)的单体可共聚合,
c)0.01-5.0重量%的至少一种交联剂,和
d)0-30重量%的一种水溶性聚合物,
a)-d)组分的总重为100%,其特征在于,该聚合物是由相对于含酸基单体部分而言,部分中和到5-30mol%的酸性聚合的单体形成,且其具有
-对0.9%NaCl水溶液,保留量至少为25g/g聚合物,
-50g/cm2压力下,吸收液体至少为25g/g聚合物,
-相对于1g聚合物的20分钟后的膨胀压至少为700g,
-16小时后的最大溶解量为3.5-10重量%,和
-最大再湿润为2.0g。
2.根据权利要求1的聚合物,其特征在于对于0.9%的NaCl水溶液,该聚合物保留值至少为30g/g聚合物,优选至少为33g/g聚合物,在50g/cm2的压力下,液体吸收至少为27%g/g聚合物,以及相对于1g聚合物,在20分钟后的膨胀压至少为850g,优选至少为900g。
3.根据权利要求1或2中任一项的聚合物,其特征在于,在20分钟后,该聚合物膨胀压至少为800g,且在2小时后,其最大膨胀压相对于20分钟后的值而言下降20%。
4.根据权利要求1-3中任一项的聚合物,其特征在于,该聚合物在16小时后具有的最大可萃取部分为3.5重量%。
5.根据权利要求1-4中任一项的聚合物,其特征在于,该水溶性聚合物是合成聚合物或共聚物和/或天然聚合物和/或天然聚合物的衍生物。
6.根据权利要求1-5的聚合物的生产方法,其特征在于,制备最大单体含量为总溶液重量的30%的水溶液;聚合反应前,该未饱和的、可聚合的含酸基的单体a)用碱中和到5.0-30mol%,优选为10-20mol%;在温度范围为5-30℃,优选为8-15℃下,用化学引发剂和/或UV辐射引发自由基聚合反应,并持续绝热;聚合物凝胶在粗磨之后,再进行粉碎,并用碱中和,以使该聚合物含有至少50mol%的聚合的、中和的含酸基单体组分;该聚合物凝胶干燥到水含量为5-20重量%,优选为≤10重量%;在温度范围为140-240℃下,干燥和研磨过的聚合物与至少一种与酸基可反应的双-或多官能交联剂反应。
7.根据权利要求6的方法,其特征在于,烯族未饱和的、可聚合的单-和/或双羧酸,优选为丙烯酸被用作未饱和的、可聚合的含酸基单体a)。
8.根据权利要求6和7的方法,其特征在于,除了含酸基单体a)外,还使用了其它水溶性的、未饱和的可聚合的单体b),其优选为丙烯酰胺,甲基丙烯酰胺,N-烷基化(甲基)丙烯酰胺,N-羟甲基(甲基)丙烯酰胺,N-乙烯基酰胺,N-乙烯基甲酰胺,N-乙烯基乙酰胺,和N-乙烯基-N-甲基乙酰胺,N-乙烯基-N-甲基甲酰胺,乙烯基吡咯烷酮,以及羟烷基(甲基)丙烯酸酯,例如羟乙基丙烯酸酯和聚乙二醇单烯丙基醚的甲基丙烯酸酯,和聚乙二醇的烯丙基醚。
9.根据权利要求6-8的方法,其特征在于,可溶或微溶于水的单体b)的使用量为全部单体重量的10%,优选为丙烯酸和甲基丙烯酸酯,例如丙烯酸乙酯和丙烯酸甲酯,醋酸乙烯酯和苯乙烯。
10.根据权利要求5-9的方法,其特征在于,用具有末端破碎孔板的挤出机进行粉碎,其孔径范围为2-20mm,优选为5-15mm,和更优选为8-13mm。
11.权利要求1-5的聚合物在吸收体液的卫生用品和在绷带中作为组成的应用。
12.权利要求1-5的聚合物在尿布,卫生巾,和失禁用品中作为组成的应用。
13.权利要求1-5的聚合物在尿布中的应用,该聚合物的重量百分含量相对于聚合物和蓬松物的重量而言为15-100%,优选为35-100%,和更优选为30-70%。
14.权利要求1-5中任一项的聚合物在电缆和光缆中作为组成的应用。
15.权利要求1-5中任一项的聚合物在土壤调节剂中作为组成的应用。
16.权利要求1-5中任一项的聚合物在用于植物培养的人造土壤中作为组成的应用。
17.权利要求1-5中任一项的聚合物在包装材料中作为组成的应用。
18.权利要求1-5中任一项的聚合物在控制释放活性物质的贮存材料中作为组成的应用。
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DE19529348A DE19529348C2 (de) | 1995-08-09 | 1995-08-09 | Absorptionsmittel für Wasser und wäßrige Flüssigkeiten auf Polyacrylatbasis sowie Verfahren zu ihrer Herstellung und Verwendung |
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-
1995
- 1995-08-09 DE DE19529348A patent/DE19529348C2/de not_active Expired - Fee Related
-
1996
- 1996-07-19 JP JP52867496A patent/JP3941880B2/ja not_active Expired - Fee Related
- 1996-07-19 WO PCT/EP1996/003203 patent/WO1997006190A1/de active IP Right Grant
- 1996-07-19 KR KR19980700863A patent/KR100441472B1/ko not_active IP Right Cessation
- 1996-07-19 US US09/000,497 patent/US6060557A/en not_active Expired - Lifetime
- 1996-07-19 EP EP96926375A patent/EP0843690B1/de not_active Expired - Lifetime
- 1996-07-19 DE DE59608767T patent/DE59608767D1/de not_active Expired - Lifetime
- 1996-07-19 CN CN96197170A patent/CN1091775C/zh not_active Expired - Fee Related
- 1996-07-19 AT AT96926375T patent/ATE213502T1/de not_active IP Right Cessation
- 1996-07-26 TW TW085109126A patent/TW434265B/zh not_active IP Right Cessation
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2000
- 2000-03-21 US US09/532,085 patent/US6403700B1/en not_active Expired - Fee Related
Also Published As
Publication number | Publication date |
---|---|
DE19529348A1 (de) | 1997-02-13 |
ATE213502T1 (de) | 2002-03-15 |
WO1997006190A1 (de) | 1997-02-20 |
TW434265B (en) | 2001-05-16 |
JP3941880B2 (ja) | 2007-07-04 |
JPH11511183A (ja) | 1999-09-28 |
EP0843690B1 (de) | 2002-02-20 |
KR19990036195A (ko) | 1999-05-25 |
CN1091775C (zh) | 2002-10-02 |
US6403700B1 (en) | 2002-06-11 |
DE19529348C2 (de) | 1997-11-20 |
US6060557A (en) | 2000-05-09 |
EP0843690A1 (de) | 1998-05-27 |
DE59608767D1 (de) | 2002-03-28 |
KR100441472B1 (ko) | 2004-10-08 |
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