CN1130386C - 使用2－噁唑烷酮的水凝胶后交联方法 - Google Patents
使用2－噁唑烷酮的水凝胶后交联方法 Download PDFInfo
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- CN1130386C CN1130386C CN99803146A CN99803146A CN1130386C CN 1130386 C CN1130386 C CN 1130386C CN 99803146 A CN99803146 A CN 99803146A CN 99803146 A CN99803146 A CN 99803146A CN 1130386 C CN1130386 C CN 1130386C
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- 238000004132 cross linking Methods 0.000 title description 7
- 238000000034 method Methods 0.000 claims abstract description 33
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- 239000004971 Cross linker Substances 0.000 claims abstract description 9
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 7
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- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 31
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 22
- 239000003795 chemical substances by application Substances 0.000 claims description 21
- 239000000126 substance Substances 0.000 claims description 17
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
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- 239000002253 acid Substances 0.000 claims description 12
- 239000003431 cross linking reagent Substances 0.000 claims description 11
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 9
- 150000008065 acid anhydrides Chemical class 0.000 claims description 7
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
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- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 4
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- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 4
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- UXFQFBNBSPQBJW-UHFFFAOYSA-N 2-amino-2-methylpropane-1,3-diol Chemical compound OCC(N)(C)CO UXFQFBNBSPQBJW-UHFFFAOYSA-N 0.000 claims description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 2
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 2
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- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 abstract description 4
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- 125000004400 (C1-C12) alkyl group Chemical group 0.000 abstract 2
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- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
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- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 3
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- FYRWKWGEFZTOQI-UHFFFAOYSA-N 3-prop-2-enoxy-2,2-bis(prop-2-enoxymethyl)propan-1-ol Chemical compound C=CCOCC(CO)(COCC=C)COCC=C FYRWKWGEFZTOQI-UHFFFAOYSA-N 0.000 description 2
- ATVJXMYDOSMEPO-UHFFFAOYSA-N 3-prop-2-enoxyprop-1-ene Chemical compound C=CCOCC=C ATVJXMYDOSMEPO-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 2
- 229920002907 Guar gum Polymers 0.000 description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 2
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- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 description 2
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- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 2
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- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 2
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- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 1
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- XHZPRMZZQOIPDS-UHFFFAOYSA-N 2-Methyl-2-[(1-oxo-2-propenyl)amino]-1-propanesulfonic acid Chemical compound OS(=O)(=O)CC(C)(C)NC(=O)C=C XHZPRMZZQOIPDS-UHFFFAOYSA-N 0.000 description 1
- LZDXRPVSAKWYDH-UHFFFAOYSA-N 2-ethyl-2-(prop-2-enoxymethyl)propane-1,3-diol Chemical compound CCC(CO)(CO)COCC=C LZDXRPVSAKWYDH-UHFFFAOYSA-N 0.000 description 1
- WFUGQJXVXHBTEM-UHFFFAOYSA-N 2-hydroperoxy-2-(2-hydroperoxybutan-2-ylperoxy)butane Chemical compound CCC(C)(OO)OOC(C)(CC)OO WFUGQJXVXHBTEM-UHFFFAOYSA-N 0.000 description 1
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- VLUWLNIMIAFOSY-UHFFFAOYSA-N 2-methylbenzenesulfinic acid Chemical compound CC1=CC=CC=C1S(O)=O VLUWLNIMIAFOSY-UHFFFAOYSA-N 0.000 description 1
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- GOXNUYXRIQJIEF-UHFFFAOYSA-N 3-(2-hydroxyethyl)-1,3-oxazolidin-2-one Chemical compound OCCN1CCOC1=O GOXNUYXRIQJIEF-UHFFFAOYSA-N 0.000 description 1
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- NJSSICCENMLTKO-HRCBOCMUSA-N [(1r,2s,4r,5r)-3-hydroxy-4-(4-methylphenyl)sulfonyloxy-6,8-dioxabicyclo[3.2.1]octan-2-yl] 4-methylbenzenesulfonate Chemical compound C1=CC(C)=CC=C1S(=O)(=O)O[C@H]1C(O)[C@@H](OS(=O)(=O)C=2C=CC(C)=CC=2)[C@@H]2OC[C@H]1O2 NJSSICCENMLTKO-HRCBOCMUSA-N 0.000 description 1
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- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
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Abstract
本发明涉及吸水性聚合物的凝胶相或表面后交联的方法，其中聚合物用表面后交联溶液处理且在处理过程中或处理之后通过升温进行后交联和干燥，交联剂是溶于惰性溶剂中的以下通式的化合物，其中R1和R2相互独立地是H、羟基、苯基或C1-C6烷基，R3是氢、C1-C12烷基、C1-C12链烯基或C6-C12-芳基，以及R4和R5相互独立地是C1-C12烷基、C1-C12链烯基、C6-C12-芳基、羟基、C1-C12-烷氧基或氢，涉及由该方法获得的吸水性聚合物，涉及该聚合物在卫生制品、包装材料和无纺织物中的用途。
Description
技术领域
本发明涉及吸水性水凝胶通过与2-噁唑烷酮共聚合来实施凝胶相或表面后交联的方法，涉及可由这种方法获得的聚合物，以及涉及它们在卫生制品、包装材料和无纺织物中的用途。
背景技术
亲水性可高度溶胀的水凝胶尤其是由(共)聚合的亲水性单体组成的聚合物，或是一种或多种亲水性单体在合适接枝基质物上的接枝(共)聚合物，交联纤维素醚或交联淀粉醚，交联羧甲基纤维素，部分交联聚亚烷基氧化物，或可在含水液体中溶胀的天然产物例如瓜耳树胶衍生物。此类水凝胶可在尿布、棉塞、卫生巾和其它卫生制品的生产中用作吸收水溶液的产品，以及用作商品蔬菜栽培中的水份保持品。
为了改进工作性能如尿布再润湿和AUL(载荷下的吸收能力)，亲水性的可高度溶胀的水凝胶一般要进行表面或凝胶相后交联。这一后交联对于本技术领域中的那些熟练人员来说是已知的并优选在含水的凝胶相中进行或以研碎的和过筛的聚合物颗粒的表面后交联方式进行。
适合此目的交联剂是包括至少两个能够与亲水聚合物的羧基形成共价键的基团的化合物。适宜交联剂的实例是二缩水甘油基或多缩水甘油基化合物如膦酸二缩水甘油基酯，烷氧基甲硅烷基化合物，聚氮丙啶，多胺和聚酰胺基胺，这些化合物还可以以相互之间的混合物使用(参见例如EP-A-0 083 022，EP-A-0 543 303和EP-A-0 530 438)。适合作为交联剂的聚酰胺基胺特别描述在EP-A-0 349 935中。
这些交联剂的一个主要缺点是它们的高反应活性，因为它必须要求在生产车间采取特殊的保护措施以避免不希望有的副作用。另外，上述交联剂具有刺激皮肤的特性，当它们用于卫生制品中时存在一些问题。
多官能醇也是已知的交联剂。例如EP-A-0 372 981，US-A-4 666 983和US-A-5 385 983讲述了亲水性多元醇的使用和多羟基表面活性剂的使用。根据这些文件，反应是在120-250℃的温度下进行的。该方法的缺点是导致交联的酯化反应甚至在此温度下仍然缓慢。
发明内容
因此，目的是，通过使用相对缓慢反应的但仍然可与羧基反应的化合物，实现良好(如果不是更好)的凝胶相或表面后交联。这一目的可通过非常短的反应时间和非常低的反应温度来实现。理想地，主反应的条件应该与使用高反应活性环氧化物时得到的那些相同。
现已令人惊奇地发现，这一目的能够通过将2-噁唑烷酮作为交联剂而以突出的效果得以实现。尤其，这些交联剂的中等反应活性能够通过添加有机或无机酸性催化剂而提高。适宜的催化剂是已知的无机酸，它们与碱金属或与铵的酸盐，以及它们的酸酐。适宜的有机催化剂是已知的羧酸，磺酸和氨基酸。
本发明提供吸水性聚合物的凝胶相或表面后交联的方法，其中聚合物用表面后交联溶液处理且在处理过程中或处理之后通过升温进行后交联和干燥，条件是交联剂是溶于惰性溶剂中的以下通式的化合物其中R1和R2相互独立地是H、羟基、苯基或C1-C6烷基，R3是氢、C1-C12-烷基、N-羟基-(C2-C6)-烷基、C1-C12-链烯基或C6-C12-芳基，以及R4和R5相互独立地是C1-C12-烷基、C1-C12-链烯基、C6-C12-芳基、羟基、C1-C12-烷氧基或氢。这一类型的优选和适宜交联剂的实例是2-噁唑烷酮，N-甲基-2-噁唑烷酮和N-羟乙基-2-噁唑烷酮。
后交联和干燥的优选温度范围是在50-250℃之间，尤其50-200℃之间，特别优选在100-180℃之间。表面后交联溶液优选通过在合适的喷射混合器中借助喷射施加到聚合物上。在喷射施加后，加热干燥聚合物粉末，有可能在干燥之前或过程中发生交联反应。在反应混合器或混合和干燥系统如Ldige混合器，BEPEX混合器，NAUTA混合器，SHUGGI混合器或PROCESSALL装置中交联剂溶液的喷射施加是优选的。而且，还有可能使用流化床干燥器。
通过加热外面的壳体或通过吹入热空气，干燥可在混合器本身中进行。同样适宜的是下游干燥器如盘架干燥机、旋转干燥器或可加热的螺杆。做为选择的措施，例如共沸蒸馏可用作干燥技术。在反应混合器或干燥器中在此温度下的优选停留时间是低于30分钟，特别优选低于10分钟。
在本发明的一个优选实施方案中，可通过向表面后交联溶液中添加酸性催化剂来加速反应。能够在本发明方法中使用的催化剂是所有的无机酸，它们的酸酐，和有机酸。实例是硼酸，硫酸，氢碘酸，磷酸，酒石酸，乙酸和甲苯磺酸。尤其合适的是它们的多聚形式、酸酐、和多元酸的酸性盐。其实例是氧化硼，三氧化硫，五氧化二磷，和磷酸二氢铵。
交联剂溶于惰性溶剂中。交联剂以基于所使用聚合物的0.01-1.0wt％的量使用。作为惰性溶剂，优选水及水与一元醇或多元醇的混合物。然而，有可能使用可与水无限混溶的任何有机溶剂，这些有机溶剂在工艺操作条件下本身不反应。当使用醇-水混合物时，该溶液的醇含量例如是10-90wt％，优选30-70wt％，尤其40-60wt％。能够使用可与水无限混溶的任何醇，并且可以是两种或多种醇的混合物(例如甲醇+甘油+水)。醇混合物包括按任何所需混合比的醇类。特别优选的是在水溶液中使用下述醇类：甲醇，乙醇，异丙醇，乙二醇和特别优选1，2-丙二醇和1，3-丙二醇。
在本发明另一个优选实施方案中，表面后交联溶液是以基于聚合物质量的1-20wt％的比例使用。特别优选的是，溶液的量基于聚合物的2.5-15wt％。
本发明另外提供可由本发明的方法获得的交联吸水性聚合物。
用于本发明方法中的亲水性可高度溶胀的水凝胶尤其是由(共)聚合的亲水性单体组成的聚合物，或一种或多种亲水性单体在合适接枝基质物上的接枝(共)聚合物，交联纤维素醚或交联淀粉醚，或可在含水液体中溶胀的天然产物例如瓜耳树胶衍生物。这些水凝胶对于本技术领域中那些熟练人员来说是已知的并描述在例如US-A-4 286 082，DE-C-27 06 135，US-A-4 340 706，DE-C-37 13 601，DE-C-28 40 010，DE-A-43 44 548，DE-A-40 20 780，DE-A-40 15 085，DE-A-39 17 846，DE-A-38 07 289，DE-A-35 33 337，DE-A-35 03 458，DE-A-42 44 548，DE-A-42 19 607，DE-A-40 21 847，DE-A-38 31 261，DE-A-35 11 086，DE-A-31 18 172，DE-A-30 28 043，DE-A-44 18 881，EP-A-0 801 483，EP-A-0 455 985，EP-A-0 467 073，EP-A-0 312 952，EP-A-0 205 874，EP-A-0 499 774，DE-A-26 12 846，DE-A-40 20 780，EP-A-0 20 5674，US-A-5 145 906，EP-A-0 530 438，EP-A-0 670 073，US-A-4 057 521，US-A-4 062 817，US-A-4 525 527，US-A-4 295 987，US-A-5 011 892，US-A-4 076 663和US-A-4 931 497中。上述专利文献的内容被特意引入本文中供参考。适合于制备这些亲水性可高度溶胀的水凝胶的亲水性单体的例子是可聚合的酸类，如丙烯酸、甲基丙烯酸、乙烯基磺酸、乙烯基膦酸、马来酸及其酸酐、富马酸、衣康酸、2-丙烯酰胺基-2-甲基丙烷磺酸、2-丙烯酰胺基-2-甲基丙烷膦酸、以及它们的酰胺，羟烷基酯，以及氨基-或铵-官能化酯和酰胺，还有含有酸基的单体的碱金属盐和/或铵盐。其它也合适的是水溶性的N-乙烯基酰胺如N-乙烯基甲酰胺或二烯丙基二甲基氯化铵。优选的亲水性单体是以下通式的化合物
其中
R1是氢，甲基或乙基，
R2是-COOR4，磺酰基，膦酰基，(C1-C4)-链烷醇-酯化的膦酰基，或下式的基团
其中
R3是氢，甲基，乙基或羧基，
R4是氢，氨基-(C1-C4)-烷基，羟基-(C1-C4)-烷基，碱金属离子或铵离子，和
R5是磺酰基，膦酰基，羧基或这些基团的碱金属盐或铵盐。
(C1-C4)-链烷醇的例子是甲醇，乙醇，正丙醇，异丙醇和正丁醇。
特别优选的亲水性单体是丙烯酸和甲基丙烯酸及其碱金属盐或铵盐，例如丙烯酸钠，丙烯酸钾或丙烯酸铵。
可通过烯属不饱和酸或它们的碱金属盐或铵盐的接枝共聚反应获得的、亲水性水凝胶的适宜接枝基质物在来源上可以是天然的或合成的。实例是淀粉、纤维素和纤维素衍生物，以及其它多糖和低聚糖，聚亚烷基氧化物，特别是聚环氧乙烷和聚环氧丙烷，和亲水性聚酯。
适宜的聚亚烷基氧化物例如具有下式其中
R6和R7相互独立地是氢，烷基，链烯基，苯基或酰基，
X是氢或甲基，和
n是1到10,000的整数。
R6和R7优选是氢，(C1-C4)-烷基，(C2-C6)-链烯基或苯基。
特别优选的水凝胶是描述在US-A-4 931 497，US-A-5 011 892和US-A-5 041 496中的聚丙烯酸盐、聚甲基丙烯酸盐和接枝共聚物。
亲水性高度可溶解的水凝胶优选是交联形式；即，它们包括具有至少两个已被共聚合到聚合物网络中的双键的化合物。特别适宜的交联剂是N，N’-亚甲基双丙烯酰胺和N，N’-亚甲基双甲基丙烯酰胺，不饱和一元或多元羧酸与多元醇的酯(如二丙烯酸酯或三丙烯酸酯)，例子是丁二醇和乙二醇的二丙烯酸酯和二甲基丙烯酸酯和三羟甲基丙烷三丙烯酸酯，以及烯丙基化合物如(甲基)丙烯酸烯丙基酯，氰尿酸三烯丙基酯，马来酸二烯丙酯，聚烯丙基酯，四烯丙氧基乙烷，三烯丙基胺，四烯丙基乙二胺，磷酸的烯丙基酯，描述在例如EP-A-0 343427中的乙烯基磷酸衍生物。然而，在本发明方法中，特别优选使用聚烯丙基醚作为交联剂和通过丙烯酸的酸性均聚反应制得的水凝胶。适宜的交联剂是季戊四醇三-和四烯丙基醚，聚乙二醇交联剂是季戊四醇三-和四烯丙基醚，聚乙二醇二烯丙基醚，单乙二醇二烯丙基醚，甘油二-和三烯丙基醚，基于山梨糖醇的聚烯丙基醚，及其乙氧基化物变体。
吸水性聚合物优选是聚合丙烯酸或聚丙烯酸盐。这一吸水性聚合物的制备是通过文献中已知的方法进行的。优选的聚合物是包括交联用共聚单体的那些(例如，含量为0.001-10，优选0.01-1mol％)。然而，非常优选的是使用多官能烯属不饱和的、另外携带至少一个游离羟基的自由基交联剂(如季戊四醇三烯丙基醚或三羟甲基丙烷二烯丙基醚)通过自由基加聚反应获得的聚合物。
亲水性可高度溶胀的水凝胶可通过常规的聚合方法制备。优选的是通过已知为凝胶聚合的一种方法在水溶液中的加聚反应。在这一方法中，例如，将一种或多种亲水性单体和如果需要的话的合适接枝基质物的15-50wt％浓度的水溶液是在自由基引发剂存在下，优选没有机械混合，利用Trommsdorff-Norrish效应(Makromol.Chem.1(1947)169)进行聚合。聚合反应可以在0℃和150℃之间，优选在10℃和100℃之间的温度范围内，在大气压力或在提高或降低的压力下进行。一般情况，聚合也可在惰性气氛下，优选在氮气中进行。聚合反应可使用高能电磁辐射或通过常规的化学聚合引发剂来引发。后者的例子是有机过氧化物，如过氧化苯甲酰，叔丁基过氧化氢，过氧化丁酮和氢过氧化枯烯，偶氮化合物，如偶氮二异丁腈，和无机过氧化合物，如(NH4)2S2O8，K2S2O8，或H2O2。如果需要，这些物质可与还原剂如连二亚硫酸钠或硫酸亚铁(II)结合使用，或与氧化还原体系结合使用。氧化还原体系包括还原性组分，它通常是脂族或芳族亚磺酸，如苯亚磺酸或甲苯亚磺酸或这些酸类的衍生物，如DE-C-1 301 566中所述的亚磺酸、醛或氨基化合物的曼尼期(Mannich)加合物。聚合物的质量能够通过进一步继续在50-130℃、优选70-100℃的温度范围内对聚合物凝胶加热几个小时而得到改进。
有可能使用常规的中和剂，优选碱金属氢氧化物或碱金属氧化物，并特别优选氢氧化钠、碳酸钠或碳酸氢钠，将所获得的凝胶中和到例如0-100mol％的程度(基于所使用的单体)，优选25-100mol％和特别优选50-85mol％。
中和通常是在中和剂中以水溶液形式或其他形式，优选以固体形式混合来进行。为此目的，凝胶利用例如破碎机进行机械粉碎，将中和剂喷射、撒布或倾倒在其上面，然后小心地混合。为了实现均化，所获得的凝胶物料再数次经过破碎机。中和的凝胶物料然后用带式干燥器或辊式干燥器进行干燥，直至残留水分含量优选低于10wt％、尤其低于5wt％为止。干燥后的水凝胶然后进行研磨和过筛，常用的研磨装置是辊式破碎机，针磨或振动球磨机。过筛后的水凝胶的优选粒度是在45-1000μm，特别优选45-850μm和非常优选200-850μm范围内。
为了确定表面后交联的质量，干燥的水凝胶然后使用下面所述的试验方法进行测试：
方法：
1)离心保留容量(CRC)：
该方法测量水凝胶在茶叶袋中的自由溶胀性。大约0.200g干燥水凝胶被密封到茶叶袋(规格：60mm×60mm，Dexter 1234T纸)中并在0.9wt％浓度的氯化钠溶液中浸泡30分钟。茶叶袋然后在常见的商购旋转干燥器(Bauknecht WS 130，1400rpm，篮子直径230mm)中旋转3分钟。液体吸收量是通过将离心的茶叶袋称重来测定的。茶叶袋本身(没有水凝胶的茶叶袋)的吸收容量通过测定空白值来予以考虑，这一空白值从称重结果(有溶胀水凝胶的茶叶袋)中扣除。
保留率CRC[g/g]＝(有水凝胶的茶叶袋称重结果-空白值-水凝胶的最初重量)/水凝胶的最初重量
2)载荷下的吸收能力(0.3/0.5/0.7psi)：
对于载荷下的吸收能力，0.900g干燥水凝胶均匀分布在测量池(measuring cell)的筛状底部(screen base)上。测量池由有机玻璃圆筒(高度＝50mm，直径＝60mm)组成，它的筛状底部是通过将圆筒底部粘接在钢丝网筛(筛孔尺寸36微米，或400目)上形成的。在均匀分布的水凝胶上放置盖板并承载适当的重量。测量池然后放置在处在多孔玻璃滤板上的滤纸(S&S 589黑带，直径＝90mm)上，而滤板本身处在含有0.9wt％浓度氯化钠溶液的陪替氏培养皿(高度30mm，直径＝200mm)中，以使在实验开始时的液面与玻璃过滤料(frit)的顶端齐平。然后让水凝胶吸收该盐溶液达60分钟。随后，从滤板上取下有溶胀凝胶的完整测量池，在取出载荷之后对装置重新称重。
载荷下的吸收能力(AUL)计算如下：
AUL[g/g]＝(Wb-Wa)/Ws其中：Wb是装置+溶胀后的凝胶两者的质量，
Wa是装置的质量+溶胀前凝胶的最初重量，和
Ws是干燥水凝胶的初始重量。
该装置是测量圆筒和盖板组成。
具体实施方式
实施例1
在40升的塑料桶中，将6.9千克的纯丙烯酸用23千克水稀释。在搅拌下向该溶液中添加45g的季戊四醇三烯丙基醚，密封的桶在通入氮气之后保持惰性。通过添加大约400mg过氧化氢和200mg抗坏血酸引发聚合反应。在反应结束后，凝胶进行机械粉碎，然后以足以达到75mol％的中和度(基于所使用的丙烯酸)的量添加氢氧化钠溶液。中和的凝胶然后在辊式干燥器上干燥，用针磨进行研磨，最后过筛分离。这是在后面的实施例中使用的基础聚合物。
在韦林氏实验室混合器中的基础聚合物用交联剂溶液进行喷射，喷射量应使得使用了5％甲醇，5％水和0.20％ 2-噁唑烷酮(基于所使用的聚合物)。随后，在循环空气干燥箱中，一部分的湿产物在170℃下处理60分钟和剩余物在170℃下处理90分钟。干燥的产物通过在850微米下过筛进行分离，以除去块状物。
实施例2
按实施例1中制备的基础聚合物在韦林氏实验室混合器中用交联剂溶液喷射。在这种情况下，该溶液具有可以达到以下剂量的组成(基于所使用的基础聚合物)：0.20wt％ 2-噁唑烷酮，5wt％丙二醇和5wt％水。湿聚合物然后在175℃分别干燥40分钟和60分钟。
实施例3
按实施例1中制备的基础聚合物在韦林氏实验室混合器中用交联剂溶液喷射。在这种情况下，该溶液具有可以达到以下剂量的组成(基于所使用的基础聚合物)：0.20wt％ 2-噁唑烷酮，5wt％丙二醇，5wt％水和0.2wt％硼酸。湿聚合物然后在175℃下干燥30分钟。
实施例4
按实施例1中制备的基础聚合物在韦林氏实验室混合器中用交联剂溶液喷射。在这种情况下，该溶液具有可以达到以下剂量的组成(基于所使用的基础聚合物)：0.20wt％ 2-噁唑烷酮，5wt％丙二醇，5wt％水和0.2wt％磷酸二氢铵。湿聚合物然后在175℃下干燥30分钟。
根据上述实施例制备的表面-后交联的聚合物按以上所述进行测试。所获得的结果总结在下表中。
这里，干燥温度和干燥时间涉及到已用表面-后交联溶液喷射的基础聚合物的热处理。
表
| 聚合物 | 干燥温度 | 干燥时间 | 催化剂 | 溶剂 | CRC[g/g] | AUL 0.3psi[g/g] | AUL 0.7psi-(4826.5Pa)[g/g] |
| 基础聚合物(按实施例1制得) | -- | -- | -- | - | 42 | 10 | 9 |
| 后交联，根据： | |||||||
| 实施例1 | 170℃ | 60分钟 | -- | 甲醇/水 | 35 | 36 | 21 |
| 实施例1 | 170℃ | 90分钟 | -- | 甲醇/水 | 32 | 34 | 27 |
| 实施例2 | 175℃ | 40分钟 | -- | 丙二醇/水 | 35 | 35 | 27 |
| 实施例2 | 175℃ | 60分钟 | -- | 丙二醇/水 | 34 | 33 | 25 |
| 实施例3 | 175℃ | 30分钟 | 0.2％ H3BO3 | 丙二醇/水 | 32 | 31 | 25 |
| 实施例4 | 175℃ | 30分钟 | 0.2％ NH4H2PO4 | 丙二醇/水 | 31 | 30 | 24 |
实施例5a
按实施例1中制备的基础聚合物在Shuggi接触器中用交联剂溶液喷射。在这种情况下，该溶液具有可以达到以下剂量的组成(基于所使用的基础聚合物)：0.20wt％ 2-噁唑烷酮，2wt％丙二醇和3wt％水。湿聚合物直接从接触器中输送至圆盘式干燥器中，在这里将产物在185℃(产物排料温度)干燥35分钟的停留时间。所获得的产物通过过筛除去较大颗粒(＞850微米)，在此之后它具有以下产品数据：CRC＝27g/g；AUL 0.7psi＝25g/g。
实施例5b
按照完全类似的方式和使用相同的设备，用下述交联剂溶液制备样品5b：4wt％丙二醇，6wt％水，0.20wt％ 2-噁唑烷酮和0.10wt％Al2(SO4)3·12-14H2O。这种产物在175℃(产物排料温度)下干燥35分钟的停留时间。所获得的产物通过过筛除去较大颗粒(＞850微米)，在此之后它具有以下产品数据：CRC＝31g/g；AUL 0.7psi＝25g/g。
实施例6
按实施例1中制备的基础聚合物在Shuggi接触器中用交联剂溶液喷射。在这种情况下，该溶液具有可以达到以下剂量的组成(基于所使用的基础聚合物)：0.10wt％ 2-噁唑烷酮，3wt％甲醇和7wt％水。湿聚合物在Nara桨式搅拌器中于185℃(产物排料温度)下干燥45分钟的停留时间。所获得的产物经过筛除去较大尺寸的颗粒(＞850微米)，在此之后它具有以下产品数据：
CRC＝26g/g；AUL 0.7psi＝25g/g.
实施例7a
按实施例1中制备的基础聚合物在实验室犁头式混合器(ProcessA1)中用交联剂溶液喷射。在这种情况下，该溶液具有可以达到以下剂量的组成(基于所使用的基础聚合物)：0.20wt％ 2-噁唑烷酮，4wt％ 1，2-丙二醇，6wt％水和0.10wt％硼酸。湿聚合物在中型试验装置流化床干燥器(Carman流化床干燥器)中在200℃(流化床温度)下干燥10分钟的停留时间。所获得的产物通过过筛除去较大颗粒(＞850微米)，在此之后它具有以下产品数据：CRC＝29g/g；AUL0.7psi＝25g/g。
实施例7b
以完全类似的方式制得的并在190℃下干燥了9分钟的停留时间的产物经过筛除去较大尺寸的颗粒(＞850微米)，在此之后它具有以下产品数据：CRC＝33g/g；AUL 0.7psi＝26g/g。
Claims (13)
1.吸水性聚合物的凝胶相或表面后交联的方法，其中聚合物用表面后交联溶液处理且在处理过程中或处理之后通过升温进行后交联和干燥，其中交联剂是2-噁唑烷酮，而吸水性聚合物是聚合丙烯酸或聚丙烯酸盐。
2.权利要求1所要求的方法，其中吸水性聚合物是通过使用多官能烯属不饱和的、可另外携带一个或多个游离羟基的自由基交联剂由自由基加成聚合反应获得的聚合丙烯酸或聚丙烯酸盐。
3.权利要求1或2中所要求的方法，其中为了进行交联使用了一种催化剂，其包含无机酸或它们的酸酐，或有机酸或它们的酸酐。
4.权利要求3中所要求的方法，其中酸是硼酸，硫酸，氢碘酸，磷酸，酒石酸，乙酸或甲苯磺酸或它们的多聚形式、酸酐或酸盐。
5.权利要求1或2中所要求的方法，其中惰性溶剂是水，水与可无限溶于水中的有机溶剂的混合物。
6.权利要求1或2中所要求的方法，其中惰性溶剂是水与一元醇或多元醇的混合物。
7.权利要求6所要求的方法，其中该溶液的醇含量是10-90wt％。
8.权利要求6所要求的方法，其中该溶液的醇含量是30-70wt％
9.权利要求6所要求的方法，其中醇是甲醇，乙醇，异丙醇，乙二醇，1，2-丙二醇或1，3-丙二醇。
10.权利要求1或2中所要求的方法，其中表面后交联溶液的用量是基于聚合物质量的1-20wt％。
11.权利要求1或2中所要求的方法，其中表面后交联溶液的用量是基于聚合物质量的2.5-15wt％。
12.由权利要求1的方法用2-噁唑烷酮表面后交联的聚合丙烯酸或聚丙烯酸盐。
13.权利要求12所要求的聚合丙烯酸或聚丙烯酸盐在卫生制品、包装材料或无纺织物中的应用。
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| DE19807502A DE19807502B4 (de) | 1998-02-21 | 1998-02-21 | Verfahren zur Nachvernetzung von Hydrogelen mit 2-Oxazolidinonen, daraus hergestellte Hydrogele und deren Verwendung |
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- 1999-02-19 CN CN99803146A patent/CN1130386C/zh not_active Expired - Lifetime
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Also Published As
| Publication number | Publication date |
|---|---|
| JP4210432B2 (ja) | 2009-01-21 |
| DE19807502B4 (de) | 2004-04-08 |
| ES2205788T3 (es) | 2004-05-01 |
| AU2927199A (en) | 1999-09-06 |
| WO1999042494A1 (de) | 1999-08-26 |
| ID25873A (id) | 2000-11-09 |
| US6472478B1 (en) | 2002-10-29 |
| BR9908006A (pt) | 2000-10-24 |
| DE19807502A1 (de) | 1999-09-16 |
| MY124251A (en) | 2006-06-30 |
| DE59906512D1 (de) | 2003-09-11 |
| CA2320778A1 (en) | 1999-08-26 |
| CN1291202A (zh) | 2001-04-11 |
| EP1056787B1 (de) | 2003-08-06 |
| EP1056787A1 (de) | 2000-12-06 |
| JP2002504566A (ja) | 2002-02-12 |
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