CN101616936A - 高吸水性聚合物在连续带式反应器上的生产 - Google Patents
高吸水性聚合物在连续带式反应器上的生产 Download PDFInfo
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- CN101616936A CN101616936A CN200880005860A CN200880005860A CN101616936A CN 101616936 A CN101616936 A CN 101616936A CN 200880005860 A CN200880005860 A CN 200880005860A CN 200880005860 A CN200880005860 A CN 200880005860A CN 101616936 A CN101616936 A CN 101616936A
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- Prior art keywords
- continuous belt
- ultraviolet lamp
- reactor
- belt reactor
- lamp modules
- Prior art date
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Abstract
本发明涉及高吸水性聚合物的生产,包括在连续带式反应器上使单体溶液聚合,其中通过调节高能量辐射的强度控制在该连续带式反应器的末端形成的聚合物凝胶的稠度。
Description
本发明涉及高吸水聚合物的生产,包括在连续带式反应器上使单体溶液聚合,其中通过调节高能量辐射的强度控制在连续带式反应器的末端形成的聚合物凝胶的稠度。
具体而言,高吸水性聚合物为(共)聚合的亲水性单体的聚合物、在合适的接枝基质上具有一种或多种亲水性单体的接枝聚合物(接枝共聚物)、纤维素或淀粉的交联醚、交联的羧甲基纤维素、部分交联的聚环氧烷,或者可在水性液体中溶胀的天然产品,例如瓜尔胶衍生物。这类聚合物被用作能够吸收水溶液的产品,以用于生产尿布、棉球、卫生棉和其他卫生用品,同时它也可用作市售园艺产品中的保水剂。
高吸水性聚合物的离心保留容量(Centrifuge Retention Capacity)一般为25至60g/g,优选地至少为30g/g,更优选地至少为32g/g,甚至更优选地至少为34g/g,最优选地至少为35g/g。离心保留容量(CRC)按照EDANA(欧洲非织布协会(European Disposables and NonwovensAssociation))推荐的No.WSP 241.2-05“离心保留容量”测试法测定。
为提高高吸水性聚合颗粒的特性如渗透性等,它们通常为后交联产物。这种后交联可在水性凝胶相进行。然而,优选地,经干燥、粉碎和筛分的基质聚合物颗粒表面包被有后交联剂,然后干燥并以热学方式进行后交联。为此目的的有用交联剂包括这样的化合物,其至少含两个能与高吸水性聚合物颗粒的羧基形成共价键或者能将基质聚合物的至少两个不同聚合链的羧基或其他官能团交联在一起的基团。
高吸水性聚合物的生产方法记载在例如专题论文“ModernSuperabsorbent Polymer Technology”,F.L.Buchholz和AT.Graham,Wiley-VCH,1998,第69-117页中。
捏合反应器或带式反应器都是合适的反应器。如WO 2001/38402A1所述,在捏合机中在水性单体溶液的聚合过程中产生的聚合物凝胶例如通过互逆搅拌杆被连续捣碎。带式反应器上的聚合在例如DE 3825366A1和US 6,241,928中均有记载。带式反应器中的聚合产生需在进一步处理步骤中在例如绞肉机、挤出机或捏合机中捣碎的聚合物凝胶。
EP 1 683 813 A1公开了在含紫外线灯的连续带式反应器上进行的高吸水性聚合物的生产。
本发明的一个目的是提供一种在一个连续带上生产高吸水性聚合物的改进方法。
我们已发现,该目的可通过一种生产高吸水性聚合物的方法实现,所述方法包括在连续带式反应器上使至少含一种光引发剂的单体溶液聚合,其中通过调节高能量辐射的强度控制该连续带式反应器末端形成的聚合物凝胶的稠度。
所述聚合通过使用至少一种光引发剂由高能量辐射作用诱导。有用的光引发剂包括例如α-分解剂(splitter)、H提取体系或叠氮化物。这类引发剂的实例有二苯甲酮衍生物如米希勒酮、菲衍生物、芴衍生物、蒽醌衍生物、噻吨酮衍生物、香豆素衍生物、苯偶姻醚及其衍生物、取代的六芳基双咪唑或酰基氧化膦,特别是2-羟基-2-甲基苯基乙基酮(1173)。叠氮化物的实例有4-叠氮基肉桂酸2-(N,N-二甲基氨基)乙酯、2-(N,N-二甲基氨基)乙基4-叠氮基萘基酮、4-叠氮基苯甲酸2-(N,N-二甲基氨基)乙酯、5-叠氮基-1-萘基2′-(N,N-二甲基氨基)乙基砜、N-(4-磺酰基叠氮苯基)马来酰亚胺、N-乙酰基-4-磺酰基叠氮苯胺、4-磺酰叠氮苯胺、4-叠氮苯胺、4-叠氮苯甲酰甲基溴化物、p-叠氮基苯甲酸、2,6-双(p-叠氮基亚苄基)环己酮和2,6-双(p-叠氮亚苄基)-4-甲基环己酮。
优选地,所述光引发剂与其他聚合引发剂联合使用。
其他有用的聚合光引发剂包括在聚合条件下可分解为自由基的所有化合物,例如过氧化物、氢过氧化物、过氧化氢、过硫酸盐、偶氮化物和氧化还原催化剂。优选使用水溶性引发剂。在某些情况下,使用多种聚合引发剂的混合物是有益的,例如使用过氧化氢与过硫酸钠或过硫酸钾的混合物。过氧化氢和过硫酸钠的混合物可以任何比例使用。有用的有机过氧化物包括例如乙酰丙酮过氧化物、甲基乙基酮过氧化物、叔丁基氢过氧化物、过氧化氢异丙苯、过新戊酸叔戊酯(tert-amylperpivalate)、过新戊酸叔丁酯、过新己酸叔丁酯(tert-butylperneohexanoate)、过异丁酸叔丁酯(tert-butyl perisobutyrate)、过-2-乙基己酸叔丁酯(tert-butyl per-2-ethylhexanoate)、过异壬酸叔丁酯(tert-butyl perisononanoate)、过马来酸叔丁酯、过苯甲酸叔丁酯、二(2-乙基己基)过氧二碳酸酯、二环己基过氧二碳酸酯、二(4-叔丁基环己基)过氧二碳酸酯、二肉豆蔻基过氧二碳酸酯、二乙酰过氧二碳酸酯、烯丙基过酸酯、过氧新癸酸枯基酯、过-3,5,5-三甲基己酸叔丁酯、乙酰基环己基磺酰基过氧化物、二月桂基过氧化物、二苯甲酰基过氧化物和过新癸酸叔戊酯。有用的聚合引发剂c)还包括水溶性偶氮引发剂,例如2,2′-偶氮双(2-脒基丙烷)二盐酸化物、2-(氨甲酰偶氮)异丁腈、2,2′-偶氮双-[2-(2′咪唑啉-2-基)丙烷]二盐酸化物和4,4′-偶氮双-(4-氰基戊酸)。所提及的聚合引发剂c)的使用量为常规量,例如,基于待聚合的单体的重量计为0.01%至5%、优选地为0.05至2.0%。
其他有用的聚合引发剂还包括氧化还原催化剂。对于氧化还原催化剂而言,氧化组分为至少一种上述过氧化物化合物,还原组分为例如抗坏血酸,葡萄糖,山梨糖,铵或碱金属的亚硫酸氢盐、亚硫酸盐、硫代硫酸盐、次硫酸盐、焦亚硫酸盐或硫化物,或者金属盐,例如亚铁离子(II)或银离子或者羟甲基次硫酸钠。氧化还原催化剂中的还原组分优选为抗坏血酸或焦亚硫酸钠。基于聚合反应中使用的单体量,氧化还原催化剂中的还原组分的使用量为1×10-5至1mol%。氧化还原催化剂中的氧化组分也可以用一种或多种水溶性偶氮引发剂替代。
形成的聚合物凝胶的稠度取决于连续带上单体的转化和干燥情况。当单体转化率低时,形成的聚合物凝胶不会吸收所有液体。这就表示在该连续带上存在两个相,即聚合物凝胶作为固相和除此之外的液相。否则,形成的低水含量的聚合物凝胶很硬,而不能沿连续带下行至连续带式反应器末端。
因此,增大高能量辐射的强度可使所形成的聚合物凝胶具有更高的单体转化率和更低的水含量;降低高能量辐射的强度可使所形成的聚合物凝胶具有更低的单体转化率和更高的水含量。
根据本发明,在连续带式反应器末端的形成的凝胶的稠度可通过变化使用的高能量辐射的强度而被控制在特定范围内。
在所述连续带式反应器末端的形成的聚合物凝胶的稠度可通过定期目测来检测。还可对形成的聚合物凝胶的弹性进行连续或半连续测量。
为防止在连续带式反应器末端的形成的聚合物凝胶固化,还可使用光垒进行控制。
高能量辐射优选为每个光子比波长为450nm的光的能量更高的辐射。紫外辐射为优选的高能量辐射。
优选地,所形成的聚合物凝胶的稠度通过调节连续带式反应器后区中高能量辐射的强度来控制。
在本发明的一个优选实施方案中,所述连续带式反应器包含至少2个紫外线灯模块。紫外线灯模块为含至少一个紫外线灯的一组紫外线灯,其中该模块的紫外线灯的强度仅能进行整体调节。这表示,例如不能只接通紫外线灯模块中两个紫外线灯中的一个。
所述连续带式反应器包含,优选至少5个,更优选至少10个,最优选至少15个紫外线灯模块。
所述紫外线灯模块的输出功率优选至少为1,000W,更优选地至少为2,500W,最优选地至少为4,000W。
使用紫外线灯模块,可通过分别接通或关闭各紫外线灯模块来调节高能量辐射的强度。
所述紫外线灯模块优选地包含至少2个紫外线灯。
在本发明的一个优选实施方案中,所述紫外线灯模块在连续带上串联排列。
连续带式反应器前区的紫外线灯模块以优选少于1m,更优选少于0.9m,最优选少于0.8m的间距排列。连续带式反应器后区的紫外线灯模块以优选至少为1m,更优选至少1.2m,最优选至少为1.4m的间距排列。上述间距为中心与中心的距离。
在本发明的一个优选实施方案中,所述连续带式反应器包含17个各自均含有2个紫外线灯的紫外线灯模块。在连续带式反应器的前区,7个紫外线灯模块以0.7m的间距排列。在连续带式反应器的后区,10个紫外线灯模块以1.5m的间距排列。
在本发明一个优选的实施方案中,聚合物凝胶下行移动至连续带式反应器的末端,并且该聚合物凝胶在下行移动过程中被旋转刀切割。
优选地,经切割的聚合物凝胶在挤出机中进一步碎裂。该挤出机可置于上述旋转刀的下方,从而使经切割的聚合物凝胶直接下落至挤出机中。
本发明的方法中可使用的单体溶液包含:
a)至少一种烯键式不饱和含酸性官能团的单体,
b)至少一种交联剂,
c)如果合适,一种或多种可与a)共聚的烯键式和/或烯丙型不饱和单体,和
d)如果合适,一种或多种在其上单体a)、b)以及合适时的c)可至少部分接枝的水溶性聚合物。
合适的单体a)为例如烯键式不饱和羧酸,如丙烯酸、甲基丙烯酸、马来酸、延胡索酸和衣康酸和/或这些酸的盐。丙烯酸和甲基丙烯酸是特别优选的单体。最优选丙烯酸。
有用的单体a)还有苯乙烯磺酸、2-丙烯酰胺基-2-甲基丙烷磺酸和2-羟基乙基丙烯酸酯。
以丙烯酸和/或其盐为代表的单体a)总量比例优选至少为50mol%,更优选至少90mol%,最优选至少95mol%。
单体a),特别是丙烯酸,优选至多包含0.025重量%的氢醌半醚。优选的氢醌半醚为氢醌一甲基醚(MEHQ)和/或生育酚。
生育酚是指下式化合物:
其中R1为氢或甲基,R2为氢或甲基,R3为氢或甲基,R4为氢或碳原子数为1-20的酸基团。
优选的R4基团为乙酰基、抗坏血酸酰基(ascorbyl)、琥珀酰基、烟酰基(nicotinyl)和其他生理学上可接受的羧酸。所述羧酸可以是一元羧酸、二元羧酸或三元羧酸。
优选R1=R2=R3=甲基的α-生育酚,特别优选外消旋α-生育酚。R4更优选为氢或乙酰基。特别优选RRR-α-生育酚。
所述单体溶液包含优选不超过130ppm重量、更优选不超过70ppm重量,优选不少于10ppm重量、更优选不少于30ppm重量、特别优选约50ppm重量的氢醌半醚,上述含量均基于丙烯酸计,其中丙烯酸盐按丙烯酸计。例如,单体溶液可使用具有合适的氢醌半醚含量的丙烯酸制备。
高吸水性聚合物为交联状态,即,在含两个或多个可聚合基团的化合物的存在下进行聚合,所述化合物可以自由基聚合的方式互相聚合成聚合物网络。有用的交联剂b)包括例如乙二醇二甲基丙烯酸酯,二乙二醇二丙烯酸酯,甲基丙烯酸烯丙酯,三羟甲基丙烷三丙烯酸酯,三烯丙基胺,EP 530 438 A1中所述的四烯丙氧基乙烷,EP 547 847 A1、EP559 476 A1、EP 632 068 A1、WO 93/21237 A1、WO 2003/104299 A1、WO 2003/104300 A1、WO 2003/104301 A1和DE 103 31 450 A1中所述的二丙烯酸酯和三丙烯酸酯,如DE 103 31 456 A1和DE 103 55 401 A1中所述的含有其他烯键式不饱和基团以及丙烯酸酯基团的混合丙烯酸酯,或者,例如DE 195 43 368 A1、DE 196 46 484 A1、WO 90/15830 A1和WO 2002/32962 A2所述的交联剂混合物。
有用的交联剂b)特别包括N,N′-亚甲基双丙烯酰胺和N,N′-亚甲基双甲基丙烯酰胺,不饱和一元羧酸或多元羧酸与多元醇的酯,例如二丙烯酸酯或三丙烯酸酯,如丁二醇二丙烯酸酯、丁二醇二甲基丙烯酸酯、乙二醇二丙烯酸酯、乙二醇二甲基丙烯酸酯,还例如,三羟甲基丙烷三丙烯酸酯以及烯丙基化合物,如(甲基)丙烯酸烯丙酯、氰脲酸三烯丙酯、马来酸二烯丙酯、聚烯丙酯、四烯丙氧基乙烷、三烯丙基胺、四烯丙基乙二胺、磷酸的烯丙酯,还例如,如EP 343 427 A2中所述的乙烯基膦酸衍生物。有用的交联剂b)还包括季戊四醇二烯丙基醚、季戊四醇三烯丙基醚、季戊四醇四烯丙基醚、聚乙二醇二烯丙基醚、乙二醇二烯丙基醚、丙三醇二烯丙基醚、丙三醇三烯丙基醚、基于山梨糖醇的聚烯丙基醚,以及它们的乙氧基化变体。本发明的方法使用聚乙二醇的二(甲基)丙烯酸酯,所使用的聚乙二醇的分子量为300至1000。
然而,特别有利的交联剂b)为3至20重(tuply)乙氧基化丙三醇的二丙烯酸酯和三丙烯酸酯、3至20重乙氧基化三羟甲基丙烷的二丙烯酸酯和三丙烯酸酯、3至20重乙氧基化三羟甲基乙烷的二丙烯酸酯和三丙烯酸酯,特别是2至6重乙氧基化丙三醇的二丙烯酸酯和三丙烯酸酯或者2至6重乙氧基化三羟甲基丙烷的二丙烯酸酯和三丙烯酸酯、3重丙氧基化丙三醇的二丙烯酸酯和三丙烯酸酯、3重丙氧基化三羟甲基丙烷的二丙烯酸酯和三丙烯酸酯,以及3重混合乙氧基化或丙氧基化丙三醇的二丙烯酸酯和三丙烯酸酯、3重混合乙氧基化或丙氧基化三羟甲基丙烷的二丙烯酸酯和三丙烯酸酯、15重乙氧基化丙三醇的二丙烯酸酯和三丙烯酸酯、15重乙氧基化三羟甲基丙烷的二丙烯酸酯和三丙烯酸酯,至少40重乙氧基化丙三醇的二丙烯酸酯和三丙烯酸酯、至少40重乙氧基化三羟甲基乙烷的二丙烯酸酯和三丙烯酸酯以及至少40重乙氧基化三羟甲基丙烷的二丙烯酸酯和三丙烯酸酯。
尤其优选用作交联剂b)的有例如WO 2003/104301 A1中所述的二丙烯酸化、二甲基丙烯酸化、三丙烯酸化或三甲基丙烯酸化的多重乙氧基化和/或丙氧基化的丙三醇。特别有利的是3至10重乙氧基化丙三醇的二或三丙烯酸酯。尤其优选1至5重乙氧基化和/或丙氧基化丙三醇的二或三丙烯酸酯。最优选3至5重乙氧基化和/或丙氧基化丙三醇的三丙烯酸酯。它们由于在吸水聚合物中的残留水平非常低(一般低于10ppm重量)而被广泛关注,通过其制备的吸水聚合物的水提取物的表面张力与相同温度下的水相比几乎没有变化(一般不少于0.068N/m)。
基于单体a)计,交联剂b)的量优选为0.001重量%至10重量%,更优选0.01重量%至5重量%,最优选0.1重量%至2重量%。
与单体a)共聚合的烯键式不饱和单体c)的实例有丙烯酰胺、甲基丙烯酰胺、丁烯酰胺、甲基丙烯酸二甲氨基乙酯、丙烯酸二甲氨基乙酯、丙烯酸二甲氨基丙酯、丙烯酸二乙氨基丙酯、丙烯酸二甲氨基丁酯、甲基丙烯酸二甲氨基乙酯、甲基丙烯酸二乙氨基乙酯、丙烯酸二甲氨基新戊酯和甲基丙烯酸二甲氨基新戊酯。
有用的水溶性聚合物d)包括聚乙烯醇、聚乙烯吡咯烷酮、淀粉、淀粉衍生物、聚乙二醇或聚丙烯酸,优选聚乙烯醇和淀粉。
单体溶液的固体含量为优选至少30重量%、更优选至少35重量%,最优选至少40重量%。所述固体含量为单体a)、交联剂b)、单体c)和聚合物d)的总和。还可使用高固体含量的水性单体悬浮液。
所述单体溶液或单体悬液在连续带上聚合形成聚合物凝胶。
所述连续带的宽度优选为1至10m,更优选为2至8m,最优选为3至6m。连续带的长度优选为3至50m,更优选为5至40m、最优选为10至30m。在连续带上的停留时间优选为5至120分钟,更优选为10至60分钟,最优选为12至40分钟。
适合于连续带的材料包括,合成树脂,例如聚乙烯树脂、聚丙烯树脂、聚酯树脂、聚酰胺树脂、氟树脂、聚氯乙烯树脂、环氧树脂、有机硅树脂、聚苯乙烯树脂、丙烯腈丁二烯苯乙烯树脂和聚氨酯树脂,以及橡胶材料,例如天然橡胶、异戊二烯橡胶、丁二烯橡胶、苯乙烯丁二烯橡胶、氯丙烯橡胶、丁腈橡胶、丙烯腈异戊二烯橡胶(nitrile isoprenerubber)、丙烯橡胶(acryl rubber)、聚氨酯橡胶、聚硫橡胶、硅橡胶和氟橡胶。在上述物质中,橡胶例如丁腈橡胶、硅橡胶和氯丙烯橡胶以及氟树脂如聚(四氟乙烯)、聚(三氟乙烯)、聚(三氟氯乙烯)和聚氟乙烯等被证明特别有利。
形成的聚合物凝胶层的厚度优选为1至20cm、更优选为2至15cm、最优选为5至10cm。然后,聚合物凝胶在另一个处理步骤,例如在绞肉机、挤出机或捏合机中被捣碎。
获得的聚合物凝胶的酸性基团通常处于部分中和状态,中和程度的范围优选为25至95mol%,更优选50至80mol%,再更优选为60至75mol%,其中可使用常规中和试剂,例如碱金属氢氧化物、碱金属氧化物、碱金属碳酸盐或碱金属碳酸氢盐,以及它们的混合物。也可使用铵盐来代替碱金属盐。钠和钾为特别优选的碱金属,最优选氢氧化钠、碳酸钠或碳酸氢钠,以及它们的混合物。
优选在单体阶段进行中和。一般通过混合呈水溶液形式、熔融物形式或优选呈固体材料形式的中和试剂进行中和作用。例如,水分数明显低于50重量%的氢氧化钠的存在形式可以是熔点高于23℃的蜡状物。此时,可以碎片物或在升高的温度下以熔融物形式进行计量。
也可在聚合作用之后在聚合物凝胶阶段进行中和。但也可在聚合之前通过向单体溶液中添加一部分中和试剂中和至多40mol%、优选10至30mol%、更优选15至25mol%的酸性基团、并在聚合后在聚合物凝胶阶段设定所需的最终中和度。聚合后聚合物凝胶至少被部分中和时,优选聚合物凝胶通过机械方式例如通过绞肉机捣碎,并且可对其喷雾、喷洒或倾注中和试剂然后将其小心混合。为此目的,可重复研磨获得的凝胶物以使其匀化。
然后优选地用带式干燥器干燥该聚合物凝胶直至残留水含量优选低于15重量%,特别地低于10重量%,水含量可通过EDANA(欧洲非织布协会)推荐的测试方法No.WSP 230.2-05“水含量”测定。或者,通过流化床干燥器或加热的犁铧混合器(plowshare mixer)进行干燥。为获得特别白的产物,通过确保蒸发水分的快速去除来干燥该凝胶非常有利。为此目的,必须对干燥器温度进行优化,还需监控空气的送入和去除,并且须保证全程时间内的充足通风。当凝胶中的固体含量尽可能高时,自然地,干燥也就更为简单并且产物也会更白。因此,干燥前凝胶的固体含量优选为30重量%至80重量%。用氮气或某些其他非氧化性惰性气体对干燥器进行通风特别有利。然而,为防止氧化变黄的过程,选择性地,也可只在干燥过程中简单地降低氧分压。但一般而言,充足的通风和去除水蒸汽同样也会获得可接受的产物。一般,很短的干燥时间对于颜色和产物质量都是有利的。
凝胶干燥的另一个重要作用是持续减少高吸水物中残留单体的含量。这是因为在干燥过程中任何残留引发剂均会分解,这就使得任何残留单体都会逐渐相互聚合。此外,蒸发的水将会夹带仍然存在的所有游离的水-蒸汽-挥发性单体,例如丙烯酸,由此降低高吸水物中的残留单体含量。
然后将干燥的聚合物凝胶研磨并分类,有用的研磨装置通常包括单级或多级轧制机(优选地包括二级或三级轧制机)、销棒粉碎机(pinmill)、锤磨机或摆动式碾磨机。
随后可将获得的聚合物进行后交联。有用的后交联剂为含两个或多个能与聚合物的羧基形成共价键的基团的化合物。有用的化合物例如为烷氧基甲硅烷基化合物、聚氮丙啶、聚胺、聚酰胺型胺类、如EP 83022A2、EP 543 303 A1和EP 937 736 A2所述的二缩水甘油基化合物(diglycidyl compound)或聚缩水甘油基化合物(polyglycidyl)、如DE 33 14 019 A1、DE 35 23 617 A1和EP 450 922 A2所述的多元醇,或者如DE 102 04 938 A1和US 6,239,230所述的β-羟烷基酰胺。也可以使用混合官能团的化合物,例如缩水甘油、如EP 1 199 327 A2中所述的3-乙基-3-氧杂环丁烷甲醇(三羟甲基丙烷氧杂环丁烷)、氨基乙醇、二乙醇胺、三乙醇胺或在初次反应后产生另一种官能团的化合物,例如,环氧乙烷、环氧丙烷、环氧异丁烷、氮丙啶、氮杂环丁烷或氧杂环丁烷。
有用的后交联剂还被认为包括DE 40 20 780 C1中所述的环状碳酸盐、DE 198 07 502 A1中所述的2-噁唑烷酮及其衍生物(例如N-(2-羟乙基)-2-噁唑烷酮)、DE 198 07 992 A1中所述的双-2-噁唑烷酮和聚-2-噁唑烷酮、DE 198 54 573 A2中所述的2-氧代四氢-1,3-噁嗪及其衍生物、DE 198 54 574 A1中所述的N-酰基-2-噁唑烷酮、DE 102 04 937 A1中所述的环状脲、DE 103 34 584 A1中所述的双环酰胺缩醛、EP 1 199 327 A2中所述的氧杂环丁烷和环状脲和WO 2003/31482 A1中所述的吗啉-2,3-二酮及其衍生物。
优选的后交联剂有噁唑烷酮及其衍生物,具体而言为N-(2-羟乙基)-2-噁唑烷酮,缩水甘油基化合物,具体而言为乙二醇二缩水甘油醚,多元醇,具体而言为甘油,以及碳酸亚乙酯。
后交联剂的量基于聚合物计优选为0.001重量%至5重量%,更优选为0.01重量%至2.5重量%,最优选为0.1重量%至1重量%。
通常,通过用后交联剂溶液、优选后交联剂水溶液喷洒聚合物凝胶或干燥的聚合物颗粒来进行后交联。喷洒后进行热干燥,在干燥前和干燥过程中均可进行后交联反应。
通过本发明的方法将聚合物与后交联剂有利地混合,并随后进行热干燥。
可通过加热混合器外壳或向其中吹入热空气在混合器中进行干燥。同样也可以使用下游干燥器,例如托盘式干燥器、旋转管式干燥箱或可加热螺杆。但也可利用例如共沸蒸馏作为干燥步骤。
优选的干燥温度为50至250℃、优选50至200℃,更优选50至150℃。在该反应混合器或干燥器中,在该温度下的优选的停留时间低于30分钟,更优选地低于10分钟。
本发明提供了一种生产高吸水性聚合物的改进方法,该方法易于控制单体转化。同时可以减少稠度的改变。这就意味着可避免过硬的聚合物凝胶在挤压机中崩解带来的例如增大输入功率和增大对轴承的压力等问题。
Claims (14)
1.一种生产高吸水性聚合物的方法,包括在连续带式反应器上使至少含一种光引发剂的单体溶液聚合,其中通过调节高能量辐射的强度控制在连续带式反应器的末端形成的聚合物凝胶的稠度。
2.权利要求1的方法,其中所述形成的聚合物凝胶的稠度通过调节该连续带式反应器后区的高能量辐射的强度而控制。
3.权利要求1或2的方法,其中所述连续带式反应器包含至少2个紫外线灯模块。
4.权利要求3的方法,其中所述紫外线灯模块包含至少两个紫外线灯。
5.权利要求3或4的方法,其中所述紫外线灯模块串联排列。
6.权利要求5的方法,其中所述连续带式反应器前区的所述紫外线灯模块以少于1m的间距排列。
7.权利要求5或6的方法,其中所述连续带式反应器的后区的紫外线灯模块以至少1m的间距排列。
8.权利要求1-7中任一项的方法,其中所述单体为至少50重量%的丙烯酸和/或其盐。
9.权利要求1-8中任一项的方法,其中所形成的聚合物凝胶被破碎。
10.一种连续带式反应器,包含至少2个紫外线灯模块。
11.权利要求10的反应器,其中所述紫外线灯模块包含至少两个紫外线灯。
12.权利要求10或11的反应器,其中所述紫外线灯模块串联排列。
13.权利要求12的反应器,其中所述连续带式反应器前区的紫外线灯模块以少于1m的间距排列。
14.权利要求12或13的反应器,其中所述连续带式反应器后区的紫外线灯模块以至少1m的间距排列。
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