CN1531613A - 用于纸张的湿强度整理剂 - Google Patents
用于纸张的湿强度整理剂 Download PDFInfo
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- CN1531613A CN1531613A CNA028117557A CN02811755A CN1531613A CN 1531613 A CN1531613 A CN 1531613A CN A028117557 A CNA028117557 A CN A028117557A CN 02811755 A CN02811755 A CN 02811755A CN 1531613 A CN1531613 A CN 1531613A
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- vinyl
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Abstract
本发明涉及用于纸张的湿强度整理剂,其含有a)1-99.9重量%的用表卤代醇交联的水溶性聚酰胺基胺和b)0.1-20重量%至少一种其他阳离子聚合物。本发明还涉及一种生产湿强度增强的纸张的方法以及所述湿强度整理剂在纸张生产过程中作为纸料的添加剂的用途。
Description
本发明涉及用于纸张的湿强度整理剂以及一种生产湿强度增强的纸张的方法。
US-A-2,926,154公开了表卤代醇与聚酰胺基胺的水溶性反应产物。该反应产物通过将其作为湿强剂加入纸料中而用于造纸。
WO-A-98/32798公开了一种聚合物组合,其通过将聚酰胺基胺与乙烯基胺聚合物的聚合物混合物用表卤代醇交联而制备。在造纸工艺中将这些反应产物加入纸料中,以增加纸张的干强度和湿强度。
US-A-4,880,497公开了含有乙烯基胺单元且通过水解N-乙烯基甲酰胺和其他烯属不饱和单体的共聚物形成的共聚物。在造纸工艺中将含有乙烯基胺单元的共聚物加入纸料中,以提高纸张的干强度和湿强度。
表卤代醇与含氨基化合物反应的反应产物具有的缺点是含有大量含氯的副产物。
本发明的目的是提供用于纸张的改进的湿强度整理剂。
我们发现该目的根据本发明通过用于纸张的湿强度整理剂实现,该整理剂包含如下组分的混合物:
(a)1-99.9重量%表卤代醇交联的聚酰胺基胺,和
(b)0.1-20重量%至少一种其他阳离子聚合物。
湿强度整理剂中的组分(b)例如为至少一种选自如下的阳离子聚合物:
-含有乙烯基胺单元的加聚物,
-未交联的聚乙烯亚胺,
-交联的聚乙烯亚胺,
-聚二烯丙基二甲基卤化铵,
-水溶性未交联的聚酰胺基胺,
-阳离子性聚丙烯酰胺,和
-双氰胺-甲醛缩合物。
特别优选包含如下组分的湿强度整理剂:
(a)表氯醇交联的水溶性聚酰胺基胺,和
(b)1-100mol%水解的聚乙烯基甲酰胺、聚乙烯和/或双氰胺-甲醛缩合物。
本发明还提供一种通过在湿强度整理剂存在下将纸料脱水而生产纸张的方法,其包括使用包含如下组分的混合物的湿强度整理剂:
(a)1-99.9重量%表卤代醇交联的水溶性聚酰胺基胺,和
(b)0.1-20重量%至少一种其他阳离子聚合物。
在该造纸方法中,将纸料与(a)表卤代醇交联的聚酰胺基胺和(b)至少一种其他阳离子聚合物同时混合或以任意顺序混合,其中所述组分(a)和(b)在任何情况下都以1-99.9∶0.1-20的重量比使用。
本发明进一步提供上述湿强度整理剂在通过在形成纸页前将其以基于干纤维为0.1-4重量%的量加入纸料中而造纸中的用途。
本发明纸张湿强度整理剂的组分(a)可以是表卤代醇交联的水溶性聚酰胺基胺。聚酰胺基胺可以通过二元羧酸与聚亚烷基多胺的缩合来制备,参见US-A-2,926,154和WO-A-98/32798。例如每摩尔二元羧酸使用0.8-1.4mol的聚亚烷基多胺。
聚酰胺基胺优选使用具有2-10个碳原子的脂族二元羧酸如草酸、丙二酸、琥珀酸、马来酸、戊二酸、己二酸、壬二酸和月桂酸来制备。优选的二元羧酸是己二酸和戊二酸。
聚亚烷基多胺的实例是二亚乙基三胺、三亚丙基四胺、四亚乙基五胺、甲基-双(3-氨基丙基)胺、二氨基丙基乙二胺、双(氨基丙基)乙二胺和氨基丙基乙二胺。
二元羧酸与聚亚烷基多胺的缩合在高温下,例如在110-220℃下进行。将缩合过程中形成的水从反应混合物中蒸除。缩合也可以在具有4-8个碳原子的羧酸的内酯或内酰胺存在下进行。与表卤代醇的反应,优选与表氯醇的反应在水溶液中于例如20-100℃,优选30-80℃下进行。聚酰胺基胺与表卤代醇的反应仅进行到所得反应产物仍溶于水中的程度为止。一旦反应溶液的粘度达到所需值,就通过加入酸如乙酸或甲酸而终止反应。这得到粘度为例如50-2000mPas,优选60-400mPas(在Brookfield粘度计中于20℃下测量,转子2,20转/分钟,聚合物水溶液浓度:12.5重量%)的表氯醇交联的聚酰胺基胺水溶液。
有用的阳离子聚合物可以衍生于例如合成和天然阳离子聚合物。有用的天然聚合物例如包括阳离子多糖、阳离子淀粉、阳离子直链淀粉及其衍生物、阳离子支链淀粉及其衍生物以及还有阳离子瓜耳胶衍生物。
合成阳离子聚合物包括例如聚乙烯亚胺。它们可以通过使乙烯亚胺在水溶液中在酸脱除化合物、酸或路易斯酸存在下聚合而制备。聚乙烯亚胺可以市购且其摩尔质量例如为200-2 000 000,优选200-1 000 000。本发明方法特别优选利用摩尔质量为500-800 000的聚乙烯亚胺。
另一类合成阳离子化合物是含有乙烯基胺单元的加聚物。它们可以由下式的开链N-乙烯基羧酰胺制备:
其中R1和R2相同或不同且各自选自氢和C1-C6-烷基。有用的单体包括例如N-乙烯基甲酰胺(在式I中R1=R2=H)、N-乙烯基-N-甲基甲酰胺、N-乙烯基乙酰胺、N-乙烯基-N-甲基乙酰胺、N-乙烯基-N-乙基乙酰胺、N-乙烯基-N-甲基丙酰胺和N-乙烯基丙酰胺。这些聚合物可以通过使所述单体单独、相互混合或与其他单烯属不饱和单体一起聚合而制备。所述加聚物优选为N-乙烯基甲酰胺的均聚物或共聚物。
用于与N-乙烯基羧酰胺共聚的有用单烯属不饱和单体包括所有可与其共聚的化合物。其实例是具有1-6个碳原子的饱和羧酸的乙烯基酯,例如甲酸乙烯基酯、乙酸乙烯基酯、丙酸乙烯基酯和丁酸乙烯基酯。有用的共聚单体还包括烯属不饱和C3-C6-羧酸,例如丙烯酸、甲基丙烯酸、马来酸、巴豆酸、衣康酸和乙烯基乙酸及其碱金属和碱土金属盐,所述羧酸的酯、酰胺和腈,例如丙烯酸甲酯、甲基丙烯酸甲酯、丙烯酸乙酯和甲基丙烯酸乙酯。其他有用的羧酸酯衍生于二醇或聚亚烷基二醇,其中在每种情况下仅一个OH被酯化,例如丙烯酸羟乙基酯、甲基丙烯酸羟乙基酯、丙烯酸羟丙基酯、丙烯酸羟丁基酯、甲基丙烯酸羟丙基酯、甲基丙烯酸羟丁基酯以及摩尔质量为500-10 000的聚亚烷基二醇的单丙烯酸酯。有用的共聚单体还包括烯属不饱和羧酸与氨基醇的酯,例如丙烯酸二甲氨基乙基酯、甲基丙烯酸二甲氨基乙基酯、丙烯酸二乙氨基乙基酯、甲基丙烯酸二乙氨基乙基酯、丙烯酸二甲氨基丙基酯、甲基丙烯酸二甲氨基丙基酯、丙烯酸二乙氨基丙基酯、丙烯酸二甲氨基丁基酯和丙烯酸二乙氨基丁基酯。碱性丙烯酸酯可以游离碱的形式,与无机酸如盐酸、硫酸或硝酸的盐形式,与有机酸如甲酸、乙酸、丙酸或磺酸的盐形式或以季铵化形式使用。有用的季铵化试剂包括例如硫酸二甲酯、硫酸二乙酯、甲基氯、乙基氯或苄基氯。
用于式I单体的有用共聚单体进一步包括烯属不饱和羧酸的酰胺,例如丙烯酰胺、甲基丙烯酰胺,以及单烯属不饱和羧酸与具有1-6个碳原子的烷基的N-烷基单酰胺和二酰胺,例如N-甲基丙烯酰胺、N,N-二甲基丙烯酰胺、N-甲基甲基丙烯酰胺、N-乙基丙烯酰胺和N-丙基丙烯酰胺和叔丁基丙烯酰胺,以及碱性(甲基)丙烯酰胺,例如二甲氨基乙基丙烯酰胺、二甲氨基乙基甲基丙烯酰胺、二乙氨基乙基丙烯酰胺、二乙氨基乙基甲基丙烯酰胺、二甲氨基丙基丙烯酰胺、二乙氨基丙基丙烯酰胺、二甲氨基丙基甲基丙烯酰胺和二乙氨基丙基甲基丙烯酰胺。
用于式I单体的有用共聚单体进一步包括N-乙烯基吡咯烷酮、N-乙烯基己内酰胺、丙烯腈、甲基丙烯腈、N-乙烯基咪唑以及取代的N-乙烯基咪唑,例如N-乙烯基-2-甲基咪唑、N-乙烯基-4-甲基咪唑、N-乙烯基-5-甲基咪唑、N-乙烯基-2-乙基咪唑,以及N-乙烯基咪唑啉类,例如N-乙烯基咪唑啉、N-乙烯基-2-甲基咪唑啉和N-乙烯基-2-乙基咪唑啉。N-乙烯基咪唑和N-乙烯基咪唑啉不仅可以以游离碱形式使用,而且可以在用无机酸或有机酸中和后或季铵化之后使用,其中季铵化优选使用硫酸二甲酯、硫酸二乙酯、甲基氯或苄基氯进行。二烯丙基二烷基卤化铵如二烯丙基二甲基氯化铵也是有用的。
用于N-乙烯基羧酰胺的有用共聚单体进一步包括含有磺基的单体,例如乙烯基磺酸、烯丙基磺酸、甲代烯丙基磺酸、苯乙烯磺酸、这些酸的碱金属盐或铵盐或丙烯酸3-磺基丙基酯。
该共聚物例如以共聚形式含有:
-99.99-1mol%式I的N-乙烯基羧酰胺,和
-1-99mol%其他可与其共聚的单烯属不饱和单体。
为了制备乙烯基胺聚合物,优选从N-乙烯基甲酰胺的均聚物或从可以通过如下单体共聚得到的共聚物开始:
-N-乙烯基甲酰胺,和
-甲酸乙烯基酯、乙酸乙烯基酯、丙酸乙烯基酯、丙烯腈或N-乙烯基吡咯烷酮,
随后水解均聚物或共聚物而由共聚的N-乙烯基甲酰胺单元形成乙酰基胺单元,其中水解度例如为1-100mol%。例如,聚乙烯基胺通过完全水解N-乙烯基甲酰胺的均聚物(水解度为100mol%)而得到。
上述聚合物的水解通过酸、碱或酶的作用并根据已知方法进行。这将上述式I的共聚的单体通过脱除下式基团:
其中R2如式I所定义,
转化成含有下式的乙烯基胺单元的聚合物:
其中R1如式I所定义。
式I的N-乙烯基羧酰胺的均聚物及其共聚物可以水解至1-100mol%的程度,有利的是水解至5-100mol%的程度,优选10-100mol%的程度。在大多数情况下,均聚物和共聚物的水解度为20-95mol%。均聚物的水解度与该聚合物的乙烯基胺单元含量含义相同。在含有衍生于乙烯基酯的单元的共聚物的情况下,N-乙烯基甲酰胺单元的水解可能伴随有酯基的水解,从而形成乙烯基醇单元。这在共聚物的水解在氢氧化钠水溶液存在下进行时尤其如此。共聚的丙烯腈同样在水解中化学改性,例如转化成酰胺基或羧基。含有乙烯基胺单元的均聚物和共聚物可以任选含有至多20mol%的脒单元,其例如通过例如共聚的N-乙烯基甲酰胺的氨基与相邻酰胺基团的分子内反应而形成。
含有乙烯基胺单元的聚合物还包括N-乙烯基甲酰胺在多糖、聚亚烷基二醇和聚乙酸乙烯基酯上的水解的接枝聚合物。接枝于聚合物上的N-乙烯基甲酰胺单元通过水解脱除甲酰基而转化成含有乙烯基胺单元的相应加聚物。含有乙烯基胺单元的接枝聚合物例如描述于US-A-5,334,287、US-A-6,048,945和US-A-6,060,566中。
在本发明的一个实施方案中,阳离子聚合物以无盐的水溶液形式或以含有不多于5重量%,优选不多于2重量%无机盐的低盐水溶液形式使用。该无盐或低盐溶液可以通过超滤或通过用有机溶剂如丙酮、甲基·乙基酮或醇沉淀中性盐而制备。
有用的阳离子聚合物进一步包括交联的聚乙烯亚胺,其例如可以通过聚乙烯亚胺与交联剂如二氯乙烯、表氯醇或具有2-100个氧化乙烯单元的聚氧化烯的双(氯乙醇)醚反应而得到。
有用的阳离子聚合物进一步包括水溶性乙烯亚胺接枝的交联聚酰胺基胺。这类缩合产物例如可根据DE-B-2 434 816通过用乙烯亚胺将聚酰胺基胺接枝并将可如此得到的乙烯亚胺接枝的聚酰胺基胺交联而得到。优选的交联剂包括具有2-100个氧化烯单元的聚氧化烯的α,ω-双(氯乙醇)醚。聚氧化烯优选衍生于氧化乙烯和/或氧化丙烯。它们可以由氧化乙烯和氧化丙烯的嵌段共聚物形成。这类产物可以市购。有用的阳离子聚合物进一步包括双氰胺-甲醛树脂,二甲胺与表氯醇的缩合产物,二甲胺与二氯链烷烃如二氯乙烷或二氯丙烷的缩合产物以及二氯乙烷与胺的缩合产物。这类反应产物例如由EP-A-0 411 400和DE-A-2 162 567已知。
有用的阳离子合成聚合物进一步包括阳离子性聚丙烯酰胺,其可以例如通过将丙烯酰胺或甲基丙烯酰胺与阳离子单体如丙烯酸或甲基丙烯酸与氨基醇的酯聚合而得到,所述酯例如为丙烯酸二甲氨基乙基酯、甲基丙烯酸二甲氨基乙基酯、丙烯酸二乙氨基乙基酯、甲基丙烯酸二乙氨基乙基酯、丙烯酸二甲氨基丙基酯和甲基丙烯酸二甲氨基丙基酯。所述碱性丙烯酸酯可以以游离碱的形式、与有机或无机酸的盐形式或以季铵化形式用于共聚中。在这类单体中,优选使用甲氯化物形式的丙烯酸二甲氨基乙基酯。用于丙烯酰胺和甲基丙烯酰胺的有用碱性共聚单体进一步包括例如丙烯酰胺基丙基三甲基铵盐和二烯丙基二甲基卤化铵。然而,也可将上述碱性共聚单体加工成均聚物并在本发明方法中用作阳离子合成聚合物。
优选的阳离子聚合物是:
-含有乙烯基胺单元的加聚物,
-聚乙烯亚胺,
-聚二烯丙基二甲基卤化铵,
-阳离子性聚丙烯酰胺,
-双氰胺-甲醛缩合物。
阳离子聚合物的摩尔质量Mw不低于15 000,优选为50 000-10 000000。阳离子聚合物的摩尔质量Mw通过光散射测定。阳离子聚合物可以具有的电荷密度为至少1.5,优选为4-15meq/g(在pH为7下测量)。
用于生产纸浆的有用纤维包括常用于该目的的所有类型,例如机械浆、漂白和未漂白的化学浆以及来自所有一年生植物的纸料。机械浆包括例如磨木浆、热法机械浆(TMP)、化学热法机械浆(CTMP)、压力磨木浆、半化学浆、高得率化学浆和盘磨机械浆(RMP)。有用的化学浆包括例如硫酸盐、亚硫酸盐和烧碱法纸浆。优选使用未漂白的化学浆,其也称为未漂白的硫酸盐浆。用于生产纸料的有用一年生植物包括例如稻、小麦、甘蔗和洋麻。纸浆也可以仅使用废纸生产或将废纸与其他纤维混合生产。废纸还包括涂布废纸,其因用于涂料和印刷油墨组合物的粘合剂含量而产生白油脂(White Pitch)。粘胶物质是因粘附标记和信封的粘合剂、粘结书脊的粘结材料以及热熔体引起的。所述纤维可以单独使用或相互混合使用。
由组分(a)和(b)组成的本发明湿强度整理剂含有例如0.1-20重量%,优选0.2-5重量%阳离子性天然和/或合成聚合物。在造纸工艺中将湿强度整理剂以0.1-5重量%,优选0.5-4重量%的量加入纸料中,其中各百分数基于干纤维。然而,组分(a)和(b)也可以在造纸工艺中以上述比例单独加入纸料中。例如可以首先将组分(a)加入纸料中,然后例如正好在流浆箱之前加入组分(b)。然而,也可以调换各组分的加入顺序;类似地,这两种组分也可以通过双组分喷嘴或通过两个单独设置的计量位置同时加入纸料中。
尽管纸张的湿强度不能通过增加加入纸料中的作为组分(a)的常规湿强剂如表氯醇交联的聚酰胺基胺的量而增加到超过一定值,但本发明的湿强度整理剂使纸张的湿强度进一步增加。
实施例中的百分数按重量计。湿断裂长度根据DIN ISO 3781在浸于水中15分钟后测定。
实施例
所用原料模型是稠度为3.3g/l的100%漂白松木硫酸盐纸浆,其被打浆至32SR且pH为7.1。将该纸浆的样品各自与表1所示的湿强剂混合并将所得混合物在每种情况下在Rapid-Kthen纸页成形器上脱水。纸页的定量在每种情况下为55g/m2。将纸页在110℃下储存5分钟。然后通过上述方法测定纸页的湿拉伸强度。所用材料和所得结果示于下表中。
湿强剂1:市售表氯醇交联的水溶性聚酰胺基胺(LuresinKNU),聚合物浓度为13.5重量%
湿强剂2:市售表氯醇交联的水溶性聚酰胺基胺(KymeneG3),聚合物浓度为16重量%
PVAm:摩尔质量Mw为400 000g/mol的聚乙烯基胺水溶液,聚合物浓度为11.8重量%
使用湿强剂1、2或PVAm时的湿断裂长度[m]
向纸料中添加 | 湿强剂1 | 湿强剂2 | PVAm | |
对比例1 | 2%Cp1) | 912m | 872m | 480m |
对比例2 | 5%CP | 1550m | 1492m | 1328m |
对比例3 | 10%CP | 2165m | 1935m | 1459m |
实施例1 | 5%CP+2%PVAm | 2161m | 2094m | - |
实施例2 | 5%CP+2%PVAm | 2030m | 1972m | - |
1)CP=市售产品
Claims (6)
1.用于纸张的湿强度整理剂,包含如下组分的混合物:
(a)1-99.9重量%表卤代醇交联的聚酰胺基胺,和
(b)0.1-20重量%至少一种其他阳离子聚合物。
2.如权利要求1所要求的湿强度整理剂,其中组分(b)为至少一种选自如下的阳离子聚合物:
-含有乙烯基胺单元的加聚物,
-未交联的聚乙烯亚胺,
-交联的聚乙烯亚胺,
-聚二烯丙基二甲基卤化铵,
-水溶性未交联的聚酰胺基胺,
-阳离子性聚丙烯酰胺,和
-双氰胺-甲醛缩合物。
3.如权利要求1或2所要求的湿强度整理剂,包含
(a)表卤代醇交联的聚酰胺基胺,和
(b)1-100mol%水解的聚乙烯基甲酰胺、聚乙烯和/或双氰胺-甲醛缩合物。
4.一种通过在湿强度整理剂存在下将纸料脱水而生产纸张的方法,包括使用包含如下组分的混合物的湿强度整理剂:
(a)1-99.9重量%表卤代醇交联的聚酰胺基胺,和
(b)0.1-20重量%至少一种其他阳离子聚合物。
5.如权利要求4所要求的方法,其中将纸料与(a)表卤代醇交联的聚酰胺基胺和(b)至少一种其他阳离子聚合物同时混合或以任意顺序混合,其中所述组分(a)和(b)在任何情况下都以1-99.9∶0.1-20的重量比使用。
6.如权利要求1-3中任一项所要求的湿强度整理剂在通过在纸页形成前以基于干纤维为0.1-4重量%的量加入纸料中而生产纸张中的用途。
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CN108026699A (zh) * | 2015-12-25 | 2018-05-11 | 星光Pmc株式会社 | 聚丙烯酰胺系造纸用添加剂和其制造方法以及纸制造方法 |
CN108179648A (zh) * | 2017-11-23 | 2018-06-19 | 湖北工业大学 | 一种提高纸张湿强度的制备方法 |
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- 2002-05-29 CN CNB028117557A patent/CN100436707C/zh not_active Expired - Fee Related
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CN108179648A (zh) * | 2017-11-23 | 2018-06-19 | 湖北工业大学 | 一种提高纸张湿强度的制备方法 |
CN108179648B (zh) * | 2017-11-23 | 2020-07-31 | 湖北工业大学 | 一种提高纸张湿强度的制备方法 |
CN114213654A (zh) * | 2021-12-31 | 2022-03-22 | 浙江百斯特化工有限公司 | 一种阳离子聚酰胺湿强剂的制备方法及其产品和应用 |
CN114213654B (zh) * | 2021-12-31 | 2023-10-20 | 浙江百斯特化工有限公司 | 一种阳离子聚酰胺湿强剂的制备方法及其产品和应用 |
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EP1399623A1 (de) | 2004-03-24 |
JP2004529279A (ja) | 2004-09-24 |
US20090008051A1 (en) | 2009-01-08 |
WO2002101144A1 (de) | 2002-12-19 |
CA2447136A1 (en) | 2002-12-19 |
US8025767B2 (en) | 2011-09-27 |
US20040149411A1 (en) | 2004-08-05 |
CN100436707C (zh) | 2008-11-26 |
EP1399623B1 (de) | 2015-01-07 |
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