CN1226261A - 水分散的共混聚合物的制备 - Google Patents
水分散的共混聚合物的制备 Download PDFInfo
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- CN1226261A CN1226261A CN97196666A CN97196666A CN1226261A CN 1226261 A CN1226261 A CN 1226261A CN 97196666 A CN97196666 A CN 97196666A CN 97196666 A CN97196666 A CN 97196666A CN 1226261 A CN1226261 A CN 1226261A
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- water
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- 239000005030 aluminium foil Substances 0.000 description 1
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- 150000004984 aromatic diamines Chemical class 0.000 description 1
- JXLHNMVSKXFWAO-UHFFFAOYSA-N azane;7-fluoro-2,1,3-benzoxadiazole-4-sulfonic acid Chemical compound N.OS(=O)(=O)C1=CC=C(F)C2=NON=C12 JXLHNMVSKXFWAO-UHFFFAOYSA-N 0.000 description 1
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- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical group OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
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- 239000011368 organic material Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
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- HJWLCRVIBGQPNF-UHFFFAOYSA-N prop-2-enylbenzene Chemical group C=CCC1=CC=CC=C1 HJWLCRVIBGQPNF-UHFFFAOYSA-N 0.000 description 1
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- 238000007342 radical addition reaction Methods 0.000 description 1
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- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 1
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- 230000007480 spreading Effects 0.000 description 1
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- 238000011105 stabilization Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- WYKYCHHWIJXDAO-UHFFFAOYSA-N tert-butyl 2-ethylhexaneperoxoate Chemical compound CCCCC(CC)C(=O)OOC(C)(C)C WYKYCHHWIJXDAO-UHFFFAOYSA-N 0.000 description 1
- WYURNTSHIVDZCO-UHFFFAOYSA-N tetrahydrofuran Substances C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 1
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- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
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Abstract
本发明涉及由聚酰胺和第二种聚合物制备水分散共混聚合物的方法,该方法使含有聚酰胺、一种或多种烯属不饱和单体、聚合引发剂,如果需要,还有乳化剂的水分散体或溶液发生聚合反应。
Description
本发明涉及聚酰胺和聚合物与烯属不饱和单体的水分散共混聚合物,还涉及它们的制备及应用。
US 4 946 932描述了制备聚酯或聚酯酰胺和由烯属不饱和单体生成的聚合物的水分散共混聚合物,而这些聚合物是通过自由基聚合制备的。这些共混聚合物应用于油漆、粘合剂或其他涂料中。这些共混聚合物的缺点是它们不会形成明亮的聚合物薄膜。这些共混聚合物的另一个缺点是聚酯或聚酯酰胺组分易发生水解,从而为共混聚合物的制备和使用设置了障碍。
US 5 277 978描述了含有硫酸酯和磺酸酯的聚酯用作稳定聚合物分散体的保护胶体。该专利建议使用以烯属不饱和单体计仅0.5-10%保护胶体。由于太大量的保护胶体可能对分散体的性能产生不利影响,所以该专利警告不要使用保护胶体的量太大。
应得到明亮、透明的薄膜。由US 4 946 932可知,当使用相对大量的聚酯时,会得到不透明的薄膜。
EP 0 687 459描述了含有带烯属不饱和单体的含水聚酯分散体的化妆组合物。该含水分散体可用于生产均匀并透明的薄膜,但只是当还加入增塑剂时才是如此。而且,这些分散体也有缺点,即由于聚酯的原因,这些分散体对水解不稳定。
本发明的一个目的是制备水分散的共混聚合物,该共混聚合物适用于涂料、化妆和药物的组合物、粘合剂,适用于织物和皮革的整理,还适用于纸张涂层,这些共混聚合物具有以下特性:
1)不需添加增塑剂可生成透明、明亮的薄膜
2)不使用增塑剂而可在常温下生成薄膜
3)使用水解稳定的聚合物
已发现,这个目的可通过制备聚酰胺和第二种聚合物的水分散的共混聚合物的方法达到的,方法中使含有聚酰胺、一种或多种烯属不饱和单体、聚合引发剂,如果需要,还有乳化剂的水分散体或溶液进行聚合。
制备水分散的共混聚合物的合适聚酰胺实际上是所有通用的水分散的和水溶性的聚酰胺。特别优选的聚酰胺由以下化合物制备得到:
a1)0-99%(摩尔)C2-C12-单氨基羧酸或其内酰胺,
a2)0.5-50%(摩尔)至少一种C2-C18-二胺,
a3)0-49%(摩尔)磺酸酯官能的C4-C12-二羧酸,和
a4)0.5-49%(摩尔)C2-C16-二羧酸。
合适的单体a1)是已知用于制备聚酰胺的单氨基羧酸,或其内酰胺,其实例是ω-氨基十一烷酸、ε-己内酰胺、月桂内酰胺、辛内酰胺或庚内酰胺。
特别合适的单体a2)是取代或未取代的脂族、环脂族或芳族二胺。合适的二胺实例是像1,2-二氨基环己烷、1,5-戊二胺、4,4’-二氨基二环己基甲烷、2,2’-(4,4’-二氨基二环己基)丙烷、3,3’-二甲基-4,4’-二氨基二环己基甲烷,或优选地六亚甲基二胺之类的亚烷基二胺或环烷基二胺。其他合适的二胺是哌嗪、2,2,4-三甲基六亚甲基二胺、2-丁基-2-乙基-1,5-戊二胺或4,7-二恶癸烷-1,10-二胺、2-甲基五亚甲基二胺和异佛尔酮二胺。
合适的磺酸酯官能单体a3)是磺酸酯基团为盐形式的那些单体,例如呈锂、钠或钾之类的碱金属盐形式,或呈未取代的或被1-4个脂族或芳族基团取代的铵基团盐形式。合适的磺酸酯官能单体是脂族或芳族二羧酸盐,例如硫代丁二酸盐或5-硫代丙氧基间苯二酸盐;优选的是使用5-硫代间苯二酸钠盐。
合适的单体a4)实例是脂族二羧酸,像癸二酸、壬二酸或十二烷二酸,或者优选地己二酸或癸二酸。合适的芳族二羧酸实例是间苯二酸或对苯二酸,它们还能是被取代的,例如3-叔丁基间苯二酸,还有3,3’-联苯基二羧酸或4,4’-联苯基二羧酸、3,3’-二苯甲烷二羧酸或4,4’-二苯甲烷二羧酸、3,3’-二苯砜二羧酸或4,4’-二苯砜二羧酸、1,4-萘二甲酸或2,6-萘二甲酸或2-苯氧基对苯二酸。
使用单体组a1)-a4)中的单个单体或同一组内多个单体的混合物这两者都是可能的。
作为水分散共混聚合物中第二种聚合物的特别合适的烯属不饱和单体是那些化合物,如有至多4个碳原子的烯烃,例如乙烯,有至多10个碳原子的乙烯基-芳族单体,例如苯乙烯、α-甲基苯乙烯、邻氯代苯乙烯或乙烯甲苯,如氯乙烯和1,1-二氯乙烯之类的卤代乙烯和卤代亚乙烯,如乙酸乙烯酯、丙酸乙烯酯、乙烯基-n-丁酸酯、月桂酸乙烯酯和硬脂酸乙烯酯之类的乙烯醇与C1-C18-一羧酸酯,优选地C3-C6-α,β-单烯属不饱和一羧酸和二羧酸,特别是丙烯酸、甲基丙烯酸、马来酸、富马酸和衣康酸,与通常C1-C12-、优选地C1-C8-、更优选地C1-C4-链烷醇的酯,特别是丙烯酸和甲基丙烯酸的甲酯、乙酯、正丁酯、异丁酸和2-乙基己基酯,马来酸二甲基酯或马来酸正丁基酯,如丙烯腈或甲基丙烯腈之类的上述的α,β-单烯属不饱和羧酸的腈,以及如1,3-丁二烯和异戊二烯之类的C4-C8共轭二烯。除单独聚合时一般可得到水溶性均聚物的单体之外的其他单体,通常包括在仅作为改性单体内,这些单体共聚时的量以使用单体的总量计是50%(重量)以下,通常是0-15%(重量),优选地1-10%(重量)。这样的单体实例是C3-C6-α,β-单烯属不饱和一羧酸和二羧酸及其酰胺,实例是丙烯酸、甲基丙烯酸、马来酸、富马酸与衣康酸、丙烯酰胺与甲基丙烯酰胺、乙烯基磺酸及其水溶性盐、乙烯基磷酸、盐及其与有至多4个碳原子的醇的酯,还有正乙烯基吡咯烷酮和丙烯酸-2-羟基乙酯、丙烯酸-3-羟基丙酯或丙烯酸二甲基氨基乙酯。
另外,单独或与下述单体组合起来使用是可能的:一种或多种乙烯基、丙烯酸和/或甲基丙烯酸单体、含硅氧烷的单体和大分子单体,还有含氟单体,例如甲基丙烯酸全氟辛酯或甲基丙烯酸-1,1,1,3,3,3-六氟异丙酯。
以使用的单体总量计,交联单体使用量是0-15%(重量),优选地是0.5-10%(重量),特别优选地是1-6%(重量);聚合物在干燥过程中,这些单体才发生交联反应,可通过热处理加速该交联反应,如果需要,可加入催化剂,例如像马来酸、磷酸氢二铵或硝酸铵之类的质子给体来加速。这样的单体实例是具有C3-C10的α,β-单烯属不饱羧酸的正醇酰胺,在这些化合物中优选的是N-羟甲基丙烯酰胺和N-羟甲基甲基丙烯酰胺。另外的交联单体是丙烯酰胺甘醇酸和甲基丙烯酰胺甘醇酸及其酯,像直到C12-链烷醇之类的醇的醚、酯或醚酯,实例是丙烯酰胺甲氧基乙酸、丙烯酰胺羟基乙酸甲酯、丙烯酰胺甲氧基乙酸甲酯、甲基丙酰酰胺甲氧基乙酸、甲基丙烯酰胺羟基乙酸甲酯、甲基丙烯酰胺甲氧基乙酸甲酯、相应的丁基和丁氧基衍生物、丙烯酰胺丁氧基乙酸丁酯和甲基丙烯酰胺丁氧基乙酸丁酯。而且,提及的(甲基)丙烯酰胺酸铵盐也是合适的。
可在有或无调节剂存在下进行自由基含水接枝聚合反应。合适的调节剂实例是巯基化合物,像巯基乙醇、巯基丙醇、巯基丁醇、巯基乙酸、巯基丙酸、丁硫醇和十二烷硫醇。其他合适的调节剂是像烯丙醇之类的烯丙基化合物。
可向聚合物分散体中加入常规的添加剂。通常在聚合反应结束后加入这些添加剂。可提及的添加剂是由不能通过聚合反应加入的交联物质,它们的使用量一般是0.1-5%(重量)。该聚合物包含游离羧基时,合适的化合物是能够使这样的基团交联的那些化合物,例如多价金属的碱性化合物,例如氧化锌、氧化钙或相应的氢氧化物、乙酸盐或碳酸盐,或者相应的混合的盐。其他合适的化合物是使任何存在的羟基交联的那些化合物,例如双官能和多官能无机酸和酸的衍生物,实例是三氯氧化磷、三偏磷酸碱金属盐、多磷酸碱金属盐或四硼酸碱金属盐,双官能和多官能有机酸,例如己二酸、柠檬酸、1,2,3,4-丁烷四甲酸、全顺-1,2,3,4-环戊烷四甲酸,双官能和多官能有机酸的衍生物,例如酐或混合的酐,实例是二乙酰基己二酸、乙酰基柠檬酸酐,像氰尿酰氯之类的酰基氯,咪唑烷和胍的衍生物,还有如1,6-己二异氰酸酯、2,4-二异氰酸根合甲苯之类的双官能和多官能异氰酸酯,如表氯醇、β,β’-二氯乙醚、双环氧化合物之类的双官能和多官能烷基化剂,如甲醛、乙醛、丙烯醛、2,5-二甲氧基四氢呋喃或戊二醛之类的醛或醛衍生物。合适的化合物还有以甲醛、乙二醛、密胺、酚和/或脲为基础的缩合物。在这些化合物中,由于醛和含醛交联剂体系的毒性问题,因而不太合适。
用于本发明制备水分散的共混聚合物的合适的聚合反应引发剂是所有能够引发自由基含水乳浊液聚合的那些化合物。它们可以是过氧化物,例如过二硫酸碱金属盐、过二硫酸铵或H2O2,也可以是偶氮化合物。
合适的还有由至少一种有机还原剂和至少一种过氧化物和/或氢过氧化构成的混合系统,实例是叔丁基过氧化氢和羟基甲烷亚磺酸钠,或者过氧化氢和抗坏血酸。混合系统也合适,该系统还包括少量溶于聚合介质的金属化合物,该金属化合物的金属组分能够以多种价态存在,该体系实例是抗坏血酸/硫酸铁(Ⅱ)/过氧化氢,这时在许多情况下抗坏血酸可用羟基甲烷亚磺酸钠、亚硫酸钠、亚硫酸氢钠或亚硫酸氢金属钠替换,过氧化氢可用叔丁基过氧化氢或过二硫酸碱金属盐和/或过二硫酸铵替换。通常,所使用的自由基引发剂体系的量,以要聚合的单体的总量计是0.1-2%(重量)。特别优选的是过二硫酸铵和/或过二硫酸碱金属盐单独或作为引发剂混合系统的组分用作引发剂。
其他合适的引发剂是如有机过氧化物之类的油溶性引发剂,实例是叔丁基过氧-2-乙基己酸酯、过碳酸酯或重氮化合物。
本发明方法可使用乳化剂或不使用乳化剂进行。合适的伴随的表面活性物质主要是通常用作分散剂用的保护胶体和乳化剂,这些物质在本质上是阴离子、阳离子或非离子的。在Houben-Weyl,Methodender organischen Chemie(有机化学方法),Volume ⅩⅣ/1,Makromolekulare Stoffe(大分子物质),Georg-Thieme-Verlag,Stuttgart,1961,411-420中详细描述了合适的保护胶体。作为伴随有表面活性的物质,优选的是仅使用乳化剂,其分子量与保护胶体不同,通常低于2000。当然,如果使用表面活性物质的混合物,混合物的各个组分必须彼此相容,如果对它们是否相容产生疑问,则可以通过几项预备试验进行检查。优选地,阴离子和非离子乳化剂用作伴随的表面活性物质。通常伴随的乳化剂实例是乙氧基化的脂肪醇(乙氧基化度(EO):3-50,烷基:C8-C36)、乙氧基化的单烷基酚、二烷基酚和三烷基酚(EO:3-50,烷基:C4-C9)、乙氧基化的链烷醇(EO:4-30,烷基:C12-C18)、乙氧基化的烷基酚(EO:3-50,烷基:C4-C9)、硫代丁二酸二烷基酯碱金属盐和硫酸烷基酯碱金属和铵盐(烷基:C8-C12)、磺酸烷基酯碱金属和铵盐(烷基:C12-C18)、烷基二苯基氧化物磺酸碱金属和铵盐(烷基:C12-C18),和烷基-芳基磺酸碱金属和铵盐(烷基:C9-C18),和相应的酸。在Houben-weyl的上述文献的192-208中给出了其他合适的乳化剂。这些表面活性物质的使用量,以待聚合单体的量计一般是0-5%(重量),优选地0.1-1%(重量)。
本发明的方法优选地用于制备共混聚合物,以聚合物总重量计,该共混聚合物含有10%(重量)以上的聚酰胺,优选地40%(重量)以上的聚酰胺。
本发明还提供用上述本发明的方法制备的水分散的共混聚合物。特别合适的共混聚合物是那些以聚合物总重量计含有聚酰胺含量为10%(重量)的共混聚合物。
这些共混聚合物适合于大量的应用,例如作为制造和整理纸张中的粘合剂,作为化妆品应用的成膜剂,具体地用于涂敷皮肤和指甲,用于药物制剂,用于生产和整理织物,用于皮革整理成膜剂,为保护金属、保护如砖石建筑与混凝土之类的无机材料、保护如木材、卡纸板、织物、涂沥青的卡纸板之类的含纤维材料或有机材料以及保护塑料用的明亮且着色的涂层材料。
本发明共混聚合物的一个明显的优点是用各种聚合物在具有高聚酰胺含量的情况下能够形成明亮的薄膜。在缩聚物与自由基加成聚合物的比例很宽的范围内都可以得到明亮的薄膜。这样一些组合物的优点是其他不相容聚合物能够按照其特性组合。这使微调水分散体的性质成为可能,因此有可能得到水可再分散的薄膜。同样可制备耐水薄膜。而且,通过聚酰胺与烯属不饱和单体的适当组合,能够得到与颜料相容的分散体;还能够得到耐溶剂的薄膜(例如耐THF的薄膜)。
另一个明显的优点是在室温下不加入增塑剂,甚至使用玻璃态转化温度远高于成膜温度的聚酰胺,也能够很好地生成薄膜。
由本发明的方法可得到的共混聚合物是平均粒度通常小于150毫微米细粒混合分散体。
通过以下实施例更详细地说明本发明。
实施例1
制备聚酰胺
将在1300毫升水中下述单体混合物装入10升实验室高压釜中:
645克5-硫代间苯二酸钠、598克间苯二酸、1116克50%浓度的六亚甲基二胺溶液、190克2,2,4-三甲基六亚甲基二胺和787克AH盐。在3小时内将该高压釜加热到200℃,在此期间通过蒸馏除去生成的水蒸气。再保持该温度不变达一小时。然后在1小时内温度升高到280℃。接着在氮气流中进行后缩合作用达2小时。然后通过一个喷咀排出熔化物,在空气床中冷却,粒化。
根据DIN 53 246(在96%H2SO4中的浓度为0.5%共聚酰胺溶液)测定,所得到聚酰胺的粘度值(VN)是45,玻璃态转化温度是143℃。
实施例2
制备聚酰胺
如实施例1所述,由840克5-硫代间苯二酸钠、521克间苯二酸、1458克浓度为50%的六亚甲基二胺溶液、710克ε-己内酰胺和1200毫升水得到聚酰胺。
该聚酰胺的玻璃态转化温度为149℃。
实施例3
制备共混聚合物
在搅拌下,将140克由实施例1得到的聚酰胺分散到850克80℃水中。然后在搅拌下,在1小时内滴加54克甲基丙烯酸甲酯和6克双丙烯酸丁二酯的混合物。接着在80℃下,在加入1毫升叔丁基过氧-2-乙基己酸酯(Trigonox 21 S d.Fa.Akzo)作为自由基引发剂之前,搅拌所得到的混合物1小时。然后进行聚合反应6小时,同时使氮通过该定量混合物。冷却得到的分散体,然后使其通过尼龙过滤器。
实施例4和5
制备共混聚合物
根据与实施例3相同的方法进行实施例4和5的操作。
聚酰胺 | 水量 | 单体 | 粒度 | 多分散性 | |
实施例4 | 140克实施例1的聚酰胺 | 850克 | 50克甲基丙烯酸甲酯+10克双丙烯酸丁二酯 | 46.2毫微米 | 0.18 |
实施例5 | 140克实施例1的聚酰胺 | 850克 | 30克丙烯酸正丁酯+30克甲基丙烯酸甲酯 | 46.1毫微米 | 0.13 |
实施例6
制备共混聚合物
将619.3克水、40克实施例2的聚酰胺、2.67克十二烷基硫酸钠(浓度为15%的溶液)和1.6克浓度为25%的氢氧化钠溶液的混合物加热到85℃,并加入5%(重量)原料流1、10%(重量)原料流2和10%(重量)原料流3。在温度85℃下进行初始聚合达15分钟,之后开始计量加入原料流1、2和3的剩余量。在2小时内(原料流1)和2.5小时内(原料流2和3)连续加入这些原料流。然后在85℃继续该聚合反应1小时。
原料流1:200克丙烯酸丁酯
200克甲基丙烯酸甲酯
原料流2:99.1克水
4克过二硫酸钠
原料流3:100克水
14.4克氢氧化钠(25%浓度)
实施例7
制备共混聚合物
将889.1克水、60克实施例2的聚酰胺、2克十二烷基硫酸钠(15%浓度的溶液)和1.2克25%浓度的氢氧化钠溶液的混合物加热到85℃,并加入5%(重量)原料流1、10%(重量)原料流2和10%(重量)原料流3。在温度85℃下进行初始聚合达15分钟,之后开始计量加入原料流1、2和3的剩余量。在2小时内(原料流1)和2.5小时内(原料流2和3)连续加入这些原料流。然后在85℃继续该聚合反应1小时。
原料流1:150克丙烯酸丁酯
150克甲基丙烯酸甲酯
原料流2:99.1克水
3克过二硫酸钠
原料流3:100克水
10.8克氢氧化钠(25%浓度)
实施例8
制备共混聚合物
将984.5克水、112克实施例2的聚酰胺、1.87克十二烷基硫酸钠(15%浓度的溶液)和1.12克25%浓度的氢氧化钠溶液的混合物加热到85℃,并加入5%(重量)原料流1、10%(重量)原料流2和10%(重量)原料流3。在温度85℃下进行初始聚合达15分钟,之后开始计量加入原料流1、2和3的剩余量。在2小时内(原料流1)和2.5小时内(原料流2和3)连续加入这些原料流。然后在85℃继续该聚合反应1小时。
原料流1:140克丙烯酸丁酯
140克甲基丙烯酸甲酯
原料流2:99.1克水
2.8克过二硫酸钠原料流3:100克水
10.1克氢氧化钠(25%浓度)
实施例9
制备共混聚合物
将1006.3克水、200克实施例2的聚酰胺、1.33克十二烷基硫酸钠(15%浓度的溶液)和0.8克25%浓度的氢氧化钠溶液的混合物加热到85℃,并加入5%(重量)原料流1、10%(重量)原料流2和10%(重量)原料流3。在温度85℃下进行初始聚合达15分钟,之后开始计量加入原料流1、2和3的剩余量。在2小时内(原料流1)和2.5小时内(原料流2和3)连续加入这些原料流。然后在85℃继续该聚合反应1小时。
原料流1:100克丙烯酸丁酯
100克甲基丙烯酸甲酯
原料流2:99.1克水
2克过二硫酸钠
原料流3:100克水
7.2克氢氧化钠(25%浓度)
实施例10
制备共混聚合物
将1606.3克水、400克实施例2的聚酰胺、1.33克十二烷基硫酸钠(15%浓度的溶液)和0.8克25%浓度氢氧化钠溶液的混合物加热到85℃,并加入5%(重量)原料流1、10%(重量)原料流2和10%(重量)原料流3。在温度85℃下进行初始聚合达15分钟,之后开始计量加入原料流1、2和3的剩余量。在2小时内(原料流1)和2.5小时内(原料流2和3)连续加入这些原料流。然后在85℃继续该聚合反应1小时。
原料流1:100克丙烯酸丁酯
100克甲基丙烯酸甲酯
原料流2:99.1克水
2克过二硫酸钠
原料流3:100克水
7.2克氢氧化钠(25%浓度)
实施例11
制备共混聚合物
将1151.8克水、40克实施例2的聚酰胺、2.67克十二烷基硫酸钠(15%浓度的溶液)和1.60克25%浓度的氢氧化钠溶液的混合物加热到85℃,并加入5%(重量)原料流1、10%(重量)原料流2和10%(重量)原料流3。在温度85℃下进行初始聚合达15分钟,之后开始计量加入原料流1、2和3的剩余量。在2小时内(原料流1)和2.5小时内(原料流2和3)连续加入这些原料流。然后在85℃继续该聚合反应1小时。
原料流1:200克丙烯酸丁酯
180克甲基丙烯酸甲酯
20克甲基丙烯酸
原料流2:99.1克水
4克过二硫酸钠
原料流3:100克水
14.4克氢氧化钠(25%浓度)
实施例12
制备共混聚合物
将1016.3克水、200克实施例2的聚酰胺、1.33克十二烷基硫酸钠(15%浓度的溶液)和0.8克25%浓度的氢氧化钠溶液的混合物加热到85℃,并加入5%(重量)原料流1、10%(重量)原料流2和10%(重量)原料流3。在温度85℃下进行初始聚合达15分钟,之后开始计量加入原料流1、2和3的剩余量。在2小时内(原料流1)和2.5小时内(原料流2和3)连续加入这些原料流。然后在85℃继续该聚合反应1小时。
原料流1:100克丙烯酸丁酯
90克甲基丙烯酸甲酯
10克甲基丙烯酸
原料流2:99.1克水
2克过二硫酸钠
原料流3:100克水
7.2克氢氧化钠(25%浓度)
实施例13
制备共混聚合物
将1131.8克水、40克实施例2的聚酰胺、2.67克十二烷基硫酸钠(15%浓度的溶液)和1.60克25%浓度的氢氧化钠溶液的混合物加热到85℃,并加入5%(重量)原料流1、10%(重量)原料流2和10%(重量)原料流3。在温度85℃下进行初始聚合达15分钟,之后开始计量加入原料流1、2和3的剩余量。在2小时内(原料流1)和2.5小时内(原料流2和3)连续加入这些原料流。然后在85℃继续该聚合反应1小时。
原料流1:400克甲基丙烯酸酯
原料流2:99.1克水
4克过二硫酸钠
原料流3:100克水
14.4克氢氧化钠(25%浓度)
实施例14
制备共混聚合物
将1006.3克水、200克实施例2的聚酰胺、1.33克十二烷基硫酸钠(15%浓度的溶液)和0.80克25%浓度的氢氧化钠溶液的混合物加热到85℃,并加入5%(重量)原料流1、10%(重量)原料流2和10%(重量)原料流3。在温度85℃下进行初始聚合达15分钟,之后开始计量加入原料流1、2和3的剩余量。在2小时内(原料流1)和2.5小时内(原料流2和3)连续加入这些原料流。然后在85℃继续该聚合反应1小时。
原料流1:200克甲基丙烯酸酯
原料流2:99.1克水
2克过二硫酸钠
原料流3:100克水
7.2克氢氧化钠(25%浓度)
实施例15
制备一种共混聚合物
将1131.8克水、40克实施例2的聚酰胺、2.67克十二烷基硫酸钠(15%浓度的溶液)和1.60克25%浓度的氢氧化钠溶液的混合物加热到85℃,并加入5%(重量)原料流1、10%(重量)原料流2和10%(重量)原料流3。在温度85℃下进行初始聚合达15分钟,之后开始计量加入原料流1、2和3的剩余量。在2小时内(原料流1)和2.5小时内(原料流2和3)连续加入这些原料流。然后在85℃继续该聚合反应1小时。
原料流1:400克乙烯基乙酸酯
原料流2:99.1克水
4克过二硫酸钠
原料流3:100克水
14.4克氢氧化钠(25%浓度)
实施例16
制备一种共混聚合物
将1006.3克水、200克实施例2的聚酰胺、1.33克十二烷基硫酸钠(15%浓度的溶液)和0.8克25%浓度的氢氧化钠溶液的混合物加热到85℃,并加入5%(重量)原料流1、10%(重量)原料流2和10%(重量)原料流3。在温度85℃下进行初始聚合达15分钟,之后开始计量加入原料流1、2和3的剩余量。在2小时内(原料流1)和2.5小时内(原料流2和3)连续加入这些原料流。然后在85℃继续该聚合反应1小时。
原料流1:200克乙酸乙烯酯
原料流2:99.1克水
2克过二硫酸钠
原料流3:100克水
7.2克氢氧化钠(25%浓度)
这些实施例的结果汇集在下表中:
实施例 | FG*) | pH | 粒度 | 多分散性 |
实施例6 | 34.2 | 7.8 | 98.8毫微米 | 0.12 |
实施例7 | 24.4 | 7.9 | 70.4毫微米 | 0.09 |
实施例8 | 24.5 | 7.7 | 75.6毫微米 | 0.26 |
实施例9 | 24.7 | 5.3 | 59.7毫微米 | 0.31 |
实施例10 | 24.4 | 4.8 | 65.7毫微米 | 0.08 |
实施例11 | 24.5 | 6.4 | 102.5毫微米 | 0.01 |
实施例12 | 23.2 | 4.3 | 57.5毫微米 | 0.27 |
实施例13 | 23.5 | 6.9 | 136.7毫微米 | 0.09 |
实施例14 | 24.4 | 4.3 | 88.7毫微米 | 0.34 |
实施例15 | 24.7 | 5.7 | 216.1毫微米 | 0.04 |
实施例16 | 24.1 | 4.9 | 147.4毫微米 | 0.15 |
*)根据DIN 53 189测定的分散体中的固体含量
实施例17
共混聚合物用作铝-纸-胶合的粘合剂
将20克水和3克增稠剂(30%(重量)浓度乳化在脂族石油馏分中的以丙烯酸和丙烯酰胺为基的共聚物水溶液)搅拌到100克例如实施例7、11或12的含水聚合物分散体中。将2克/平方米(干的)这种胶合粘合剂涂到厚0.015毫米铝箔的一个无光泽面上。把黄杨碱纸(80克/平方米)辗压到粘合剂湿层上,在50℃将其干燥3分钟。接着将以这种方法得到的基片切成200毫米×30毫米大小,24小时后进行测试。
发现铝-纸粘合体具有良好强度。
实施例18
共混聚合物用作无纺物的粘合剂
使用的粘合剂是按照实施例6-10用96%(重量)丙烯酸乙酯和4%(重量)丙烯酰胺甘醇酸制备的聚合物,其固体含量为45%。
根据已知方法(Ullmann’s Enzyklopdie der technischenChemie(工业化学百科全书),第4版,23卷,1983,738-742)把纤维织物用聚合物固结。织物处理后,干燥和加热该织物,以得到粘合的纤维织物。
得到具有良好使用性能的无纺物。
实施例19
用作头发定型剂
(百分比为重量百分比)
定型剂配方1
25%实施例4的水分散体
0.2%芳香油、着色剂和防腐剂
74.8%水
将这些物质混合。
定型剂配方2
15%实施例5的水分散体
1.5%60%(重量)N-乙烯基吡咯烷酮和40%(重量)乙酸乙
烯酯的共聚物
0.2%芳香油、着色剂和防腐剂
83.3%水
将这些物质混合。
得到的制剂显示了良好的定型效果。
实施例20
用作指甲油
(百分比是重量百分比)
75%实施例6的分散体与1%颜料和24%水混合。
得到有光泽、粘合良好的薄膜。
实施例21
纸张涂层组合物的粘合剂
60%(重量)浓度的纸张涂敷颜料含有
80克瓷土5PS(高岭土)
20克Omyalite 90(白垩)
0.2克PolysalzS(低分子质量聚丙烯酸,高岭土和白
垩的分散剂)
11.5克实施例6-10的水分散体(以干燥状态计),含
55%(重量)丙烯酸正丁基酯、43%(重量)甲基丙烯
酸甲酯和2%(重量)丙烯酸,固体含量为50%。
0.6克BlankophorPSG-fl.(荧光增白剂)和
0.3克SterocollD(以干基计),(富丙烯酸的丙烯酸
酯聚合物的水分散体,增稠剂)
水
得到具有良好涂敷性能的纸张涂敷组合物。
Claims (11)
1.一种由聚酰胺和第二种聚合物制备水分散共混聚合物的方法,该方法是使含有聚酰胺、一种或多种烯属不饱和单体、聚合引发剂,如果需要,还有乳化剂水分散体或溶液进行聚合反应。
2.根据权利要求1所述的方法,其特征在于该共混聚合物含有10%(重量)以上的聚酰胺。
3.根据权利要求1所述的方法,其特征在于该聚酰胺由以下化合物构成:
a1)0-99%(摩尔)C2-C12-单氨基羧酸或其内酰胺,
a2)0.5-50%(摩尔)至少一种C2-C18-二胺,
a3)0-49%(摩尔)磺酸酯官能C4-C12-二羧酸,和
a4)0.5-49%(摩尔)C2-C16-二羧酸。
4.根据权利要求1所述的方法,其特征在于第二种聚合物由单体丙烯酸正丁基酯、甲基丙烯酸甲酯或甲基丙烯酸或其混合物组成。
5.根据权利要求1-4之任一权利要求所述方法得到的水分散共混聚合物。
6.根据权利要求5所述的共混聚合物用于纸涂层。
7.根据权利要求5所述的共混聚合物用于化妆品配方。
8.根据权利要求7所述的共混聚合物的应用,其特征在于该共混聚合物是用于头发护理剂。
9.根据权利要求7所述的共混聚合物的应用,其特征在于该共混聚合物是用于指甲油。
10.根据权利要求5所述的共混聚合物用作粘合剂。
11.根据权利要求5所述的共混聚合物用作无纺物的粘合剂。
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DE19629452.5 | 1996-07-23 | ||
DE19629452A DE19629452A1 (de) | 1996-07-23 | 1996-07-23 | Verfahren zur Herstellung wasserdispergierbarer Polymerblends |
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JP (1) | JP2000514814A (zh) |
KR (1) | KR20000067991A (zh) |
CN (1) | CN1226261A (zh) |
AU (1) | AU3543697A (zh) |
BR (1) | BR9710524A (zh) |
CA (1) | CA2260822A1 (zh) |
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WO (1) | WO1998003567A1 (zh) |
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CN101300281B (zh) * | 2005-11-03 | 2012-11-14 | 巴斯夫欧洲公司 | 具有梳状稳定剂的水溶性聚合物的水分散体 |
CN106893046A (zh) * | 2017-04-11 | 2017-06-27 | 江苏泰格油墨有限公司 | 一种尼龙水性分散体及其制备方法 |
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FR2793800A1 (fr) * | 1999-05-21 | 2000-11-24 | Atofina | Dispersions aqueuses de polyamides et de polymeres vinyliques et/ou acryliques |
JP4217341B2 (ja) * | 1999-05-24 | 2009-01-28 | 日本化薬株式会社 | 芳香族ポリアミド樹脂組成物 |
DE102005005493A1 (de) * | 2005-02-04 | 2006-08-10 | Basf Ag | Verfahren zur Herstellung einer wässrigen Polymerdispersion |
DE102005016226A1 (de) * | 2005-04-07 | 2006-10-12 | Basf Ag | Verfahren zur Herstellung einer wässrigen Polymerdispersion |
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US4946932A (en) * | 1988-12-05 | 1990-08-07 | Eastman Kodak Company | Water-dispersible polyester blends |
WO1995001381A1 (en) * | 1993-06-29 | 1995-01-12 | Eastman Chemical Company | Polymer blends comprising sulfonate group-containing surfactants |
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1996
- 1996-07-23 DE DE19629452A patent/DE19629452A1/de not_active Withdrawn
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1997
- 1997-07-14 CA CA002260822A patent/CA2260822A1/en not_active Abandoned
- 1997-07-14 WO PCT/EP1997/003754 patent/WO1998003567A1/de not_active Application Discontinuation
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CN101300281B (zh) * | 2005-11-03 | 2012-11-14 | 巴斯夫欧洲公司 | 具有梳状稳定剂的水溶性聚合物的水分散体 |
CN106893046A (zh) * | 2017-04-11 | 2017-06-27 | 江苏泰格油墨有限公司 | 一种尼龙水性分散体及其制备方法 |
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WO1998003567A1 (de) | 1998-01-29 |
DE19629452A1 (de) | 1998-01-29 |
BR9710524A (pt) | 1999-08-17 |
CA2260822A1 (en) | 1998-01-29 |
JP2000514814A (ja) | 2000-11-07 |
EP0914359A1 (de) | 1999-05-12 |
KR20000067991A (ko) | 2000-11-25 |
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