CN1094422A - 粘合有糖化物接枝聚合物的可堆肥的无纺织物 - Google Patents
粘合有糖化物接枝聚合物的可堆肥的无纺织物 Download PDFInfo
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- CN1094422A CN1094422A CN93114659A CN93114659A CN1094422A CN 1094422 A CN1094422 A CN 1094422A CN 93114659 A CN93114659 A CN 93114659A CN 93114659 A CN93114659 A CN 93114659A CN 1094422 A CN1094422 A CN 1094422A
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- Prior art keywords
- acid
- nonwoven fabric
- ester
- water
- polymkeric substance
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- 239000000178 monomer Substances 0.000 claims abstract description 39
- 239000000126 substance Substances 0.000 claims abstract description 21
- 239000000835 fiber Substances 0.000 claims abstract description 20
- 150000002148 esters Chemical class 0.000 claims abstract description 19
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 14
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- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 10
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- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 8
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- LPQOADBMXVRBNX-UHFFFAOYSA-N ac1ldcw0 Chemical compound Cl.C1CN(C)CCN1C1=C(F)C=C2C(=O)C(C(O)=O)=CN3CCSC1=C32 LPQOADBMXVRBNX-UHFFFAOYSA-N 0.000 claims description 5
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- FKRCODPIKNYEAC-UHFFFAOYSA-N ethyl propionate Chemical compound CCOC(=O)CC FKRCODPIKNYEAC-UHFFFAOYSA-N 0.000 claims description 2
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- 229910000360 iron(III) sulfate Inorganic materials 0.000 description 9
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 8
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- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 7
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- 239000003995 emulsifying agent Substances 0.000 description 7
- QMMOXUPEWRXHJS-UHFFFAOYSA-N pent-2-ene Chemical group CCC=CC QMMOXUPEWRXHJS-UHFFFAOYSA-N 0.000 description 7
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- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 5
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 5
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 4
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 4
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- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 4
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Classifications
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/285—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acid amides or imides
- D06M15/29—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acid amides or imides containing a N-methylol group or an etherified N-methylol group; containing a N-aminomethylene group; containing a N-sulfidomethylene group
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- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/22—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing macromolecular materials
- A61L15/225—Mixtures of macromolecular compounds
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- A—HUMAN NECESSITIES
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- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/42—Use of materials characterised by their function or physical properties
- A61L15/62—Compostable, hydrosoluble or hydrodegradable materials
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
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- D—TEXTILES; PAPER
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Abstract
适用于堆肥的无纺织物,按所用纤维重量计,粘
合有5—100%(wt)的玻璃化温度为-70——40℃的
聚合物,该聚合物通过在有糖化物存在的水介质中对
烯键不饱和单体的混合物进行自由基聚合反应而获
得,单体混合物含有0.5—15%(wt)单烯键不饱和的
有3—10个碳原子的羧酸、丙烯酰胺乙醇酸、甲基丙
烯酰胺乙醇酸的N-醇酰胺和/或其与具有达12个
碳原子之醇类形成的醚和酯或醚-酯。
Description
本发明涉及粘合有5-100%(按所用纤维重量计)聚合物的无纺织物。所说的聚合物具有玻璃化温度为-70-+40℃,且在有糖化物存在下可在水介质中由烯键不饱和单体的自由基聚合进行制备。
无纺织物通常是用凝固或粘合松散的各个纤维的堆积物即纤维网所形成的柔性纺织片状材料,通过用聚合物分散水溶液浸渍以及随后进行蒸发水份来凝固或粘合纤维网以形成粘合的纤维网即无纺织物通常为已知技术。
与机织和针织织物相比较,由于无纺织物生产比较便宜,所以在一次性纺织品方面具有广泛的应用前景,例如尿布、抹布及医用品如卫生毛巾或罩布及卫生套。
这些产品不仅在干燥状态下而且在潮湿状态下一般都需要具有高强度,同时具有柔软特性。另外,对于那些或多或少与人有直接接触的产品,则在其毒性安全方面必须满足更高的要求。
随着这些一次性产品用量的增加,人类社会变得比以往任何时候都更加关心废物问题,其兴趣开始集中在如何处理用过的产品。至今为止,处理办法主要是填埋。其结果是填埋空间变少,填埋本身以政治上考虑也难以被接受,所以用理想的堆肥法来处理含有无纺织物的一次性用品是非常需要的。因此,产品应该是容易堆肥的,即在堆肥池中充分地腐烂掉。当与土壤接触时,产品应该迅速失去其强度并且分解。
DE-A-2361468介绍一种由短纤维如纤维素纤维和粘合剂组成的无纺织物,粘合剂含有烯键不饱和单体聚合物和天然生成聚合物如明胶、胶原或淀粉的混合物,将混合物施加到纤维网上,除去其中的水溶性介质和水份。但是,用上述方法制得的无纺织物不能令人满意,问题在于这种无纺织物具有不良特性。例如,这种产品的柔软性和湿强度不好。
US-A-3651210描述了一种尤其含环氧乙烷的单体和作为涂复材料或粘合剂的蛋白质如酪蛋白或豆蛋白的活性共聚物。德国专利申请P4108170.6公开了有蛋白质如酪蛋白存在的自由基聚合烯键不饱和单体乳液。该产品用于生产薄膜和涂覆材料如纸表面涂层。但没有一篇参考文献报道采用在有淀粉作粘合纤维网粘合剂存在下制备聚合物的任何报道。此外,P4108170.6介绍的用接枝聚合物作粘结剂制备的无纺织物不能彻底防水,而且过硬。
EP-A-345566涉及基于无羟基单体和含羟成分如聚乙烯醇、淀粉、淀粉衍生物或胶态纤维素之共聚物的网粘合剂。这些网粘合剂可通过向聚合物中加入1,3-二甲基-4,5-二羟咪唑酮进行交联。但是,这些产品的湿强度差,且柔软性不理想。
本发明的目的是避免上述现有技术中所存在的缺陷,提供具有平衡特性及可堆肥的无纺织物。该产品应具有高干强度、好的湿强度和柔软性及易堆肥的综合特性。
我们发现,本发明的目的可由在本发明说明书开头所定义的无纺织物获得。我们也发现了凝固纤维网的方法。在从属权利要求中描述了优选的方案。
作为纤维网的合适材料是生物可降解纤维,这通常是具有直径为0.002-0.1mm、优选为0.01-0.05mm的纤维,可采传统方法电子显微方式进行测量。所用的纤维一般为纤维素源的天然纤维如粘胶纤维或纤维素纤维,或合成纤维如脂肪族聚酯纤维,例如基于3-羟丁酸酯、3-羟戊酸酯和4-羟戊酸酯之共聚物的聚酯纤维(参见EP-A-466050)。
用纤维制成纤维网属于一般技术(Rompp,Chemielexikon,Georg Thieme Verlag,Stuffgart-New Nork,9th Edition,P.4560)。它们可以是无规则铺置的纤维网,较好的是有或无机械预定型如针刺、缠结或针缝的取向纤维网。
纤维网与按所用纤维网重量计为5%以上、较好11%以上、尤其15%以上、特别20%以上且100%以下、较好50%以下、尤其35%以下的聚合物粘合。
将烯键不饱和单体接枝到淀粉上的方法是已知的,如EP-A-134449、EP-A-334515、EP-A-408099和德国专利申请P4133193.1所介绍的。淀粉接枝聚合物被推荐作纸上浆用(EP-A-257412),作为清洗剂或纸涂覆成分的配合物(EP-A-441197),作为金属铸造用的模(德国专利申请P4133190.7)和磨料(德国专利申请P4133191.5)。
根据本发明所用的聚合物具有玻璃化温度-70-40℃,较好的为-60-0℃。这玻璃化温度可按传统方法测量,按美国材料试验学会(ASTM)3418/82(中点温度)所述方法进行。
合适的自由基聚合单体主要是单烯键不饱和单体,例如达4个碳原子的烯烃类象乙烯、达10个碳原子的芳香基乙烯单体象苯乙烯、α-甲基苯乙烯、邻氯苯乙烯或乙烯基甲苯类、乙烯基和亚乙烯基卤代物象乙烯基氯和亚乙烯基氯、乙烯醇与1-18个碳原子单羧酸的酯类象乙烯基乙酸酯、乙烯基丙酸酯、乙烯基正丁酸酯、乙烯基月桂酸酯和乙烯基硬脂酸酯、单烯键不饱和的含较好为3-6个碳原子的单和二羧酸尤其为丙烯酸、甲基丙烯酸、马来酸、富马酸及衣康酸与含有一般为1-12、较好为1-8、最好为1-4个碳原子的醇形成的酯类,尤其是丙烯酸甲酯、丙烯酸乙酯、丙烯酸正丁酯、丙烯酸异丁酯、丙烯酸2-乙基己酯、异丁烯酸甲酯、异丁烯酸乙酯、异丁烯酸正丁酯、异丁烯酸异丁酯及异丁烯酸2-乙基己酯、马来酸二甲酯或马来酸正丁酯、所说的单烯键不饱和和羧酸的腈类,如丙烯腈或甲基丙烯腈,还有C4-C8共轭二烯类如1,3-丁二烯及异戊二烯。在很多情况下按所用单体总重量计腈类比例占15%以下,较好的是0%为好。
所说的单体基本上是不溶于水介质的,而且一般为主体单体,按所用单体总量计其比例通常占50%以上。
按所用单体总重量计,采用交联单体的量为0.5-15%、较好为0.5-10%、最好为1-6%,在聚合物被干燥之前不要对单体进行交联,而后在有或无催化剂存在下通过加热使交联反应加速,所说的催化剂如质子除去物质象马来酸、磷酸氢二铵或硝酸铵。这类单体的例子有3-10个碳原子单烯键不饱和羧酸的正醇酰胺,其中N-羟甲基丙烯酰胺和N-羟甲基甲基丙烯酰胺是优选的。用作交联单体特别优选的是丙烯酰胺乙醇酸和甲基丙烯酰胺乙醇酸及其酯类,与醇如达12个碳原子醇类形成的酯或乙酯,例如丙烯酰胺甲氧基乙酸、甲基丙烯酰胺羟基乙酸酯、甲基丙烯酰胺甲氧基乙酸酯、甲基丙烯酰胺甲氧基乙酸、甲基异丁烯酰胺羟基乙酯、甲基异丁烯酰胺甲氧基乙酯,相应的丁基和丁氧基衍生物、丁基丙烯酰胺丁氧基乙基和丁基甲基丙烯酰胺丁氧基乙酯。所说的甲基丙烯酰胺酸的铵盐也是合适的。这种交联方法在交联反应中根本不放出任何有毒的甲醛。无甲基丙烯酰胺乙醇酸是特别优选的。
其它的通过自身聚合的通常产生水溶性均聚物的单体只按改性的量加入到共聚物中,加入的量按所用单体总量计为50%以下,一般为0-15%,较好为1-10%。这类单体的例子是具有3-6个碳原子的单烯键不饱和单和双羧酸及其酰胺,如丙烯酸、甲基丙烯酸、马来酸、富马酸、衣康酸、丙烯酰胺和甲基丙烯酰胺,还有乙烯磺酸及其水溶性盐、乙烯磷酸、其与含有达4个碳原子的醇形成的盐和酯、以及N-乙烯吡咯烷酮和2-羟乙基丙烯酸酯、3-羟丙基丙烯酸酯或二甲基氨乙基丙烯酸酯。
优选的聚合物为:
70-99.5%(wt)丙烯酸和/或甲基丙烯酸与具有1-12个碳原子醇形成的酯、苯乙烯、丁二烯、乙烯基乙酸酯和/或丙酸酯;
0.5-15%(wt)交联单体,和
0-15%(wt)其它单体。
特别优选的聚合物选自含有90-99.5%(wt)、较好为94-99%(wt)丙烯酸和/或甲基丙烯酸与具有1-12个特别为1-8个碳原子醇形成的酯类与0.5-10%(wt)、较好1-6%(wt)丙烯酸、甲基丙烯酸和/或最好为丙烯酰胺乙醇酸、甲基丙烯酰胺乙醇酸的单体混合物,以及上述这些酸类的衍生物,其中丙烯酰胺乙醇酸和甲基丙烯酰胺乙醇酸为特别优选的。
所提到的各重量百分比是按所用烯键不饱和单体的总量计算的。
所说的单体一般按自由基水乳液聚合法进行聚合,实际上是一种在糖化物存在下的接枝聚合。用于本发明方法的糖化物为单糖、低聚糖、多糖及其衍生物。
单糖包括戊糖(C5H10O5)和已糖(C6H12O6)。低聚糖如单糖的二聚物或三聚物。较好的是采用单糖和低聚糖的衍生物,如具有C6-C18醇的乙缩醛。合适的是辛基-D-葡糖苷、癸基-D-葡糖苷、十二烷基-D-葡糖苷、十四烷基-D-葡糖苷、十六烷基-D-葡糖苷、十八烷基-D-葡糖苷及其混合物。
所用的多糖优选为配糖键合的多糖。
优选的多糖平均分子重量为1000-25000,较好为1000-13000,最好为2000-9000,可按传统方式用凝胶渗透色谱法进行测量。
多糖可以是植物或动物多糖,为水溶性或仅为水分散性的。其中合适的是膨胀淀粉,这类淀粉可用湿热处理天然淀粉获得。薄膜蒸发淀粉也是合适的。这类淀粉是可以用酸或酶进行轻度降解,或用轻度氧化剂进行氧化,当用水煮沸时根本不形成粘胶,既便在很高浓度情况下也保持相对薄的液体。也可以用酸改性淀粉,它可以在有少量酸存在下于胶化温度以下通过加热水淀粉悬浮液进行制备。氧化改性淀粉也是合适的。合适的氧化剂包括如铬酸、高锰酸盐、过氧化氢、二氧化氢、氢氯化物或高碘酸。原则上讲原料淀粉可以是任何一种天然淀粉,如谷物淀粉(象玉米、小麦、稻谷或小淀粉)、块茎类淀粉或植根淀粉(象土豆、木薯淀粉或木薯粉)或西谷米淀粉。较好的是采用如EP-A-408099和EP-A-334515介绍的焙烧糊精,通常在有少量酸存在下通过加热湿干淀粉获得该类糊精。典型的焙烧糊精为如工业上可获得的白和黄糊精,也包括商标为Noredux和Tackidex的糊精。在此术语糊精通常是指淀粉降解产品。
然而,在有糖化淀粉存在下进行自由基乳液聚合是非常好的。这些是在水相用水解法获得的淀粉降解产品。生成物水聚合分散液,除了具有高机械和热稳定性外,既使在贮存后也有很好的流变性质。所说的淀粉及淀粉衍生物的具体制备方法可参见G.Tegge,Starke and Starkederivate,Behr′s Verlag,Hamburg 1984。当然,所说的淀粉及其衍生物经过化学改性如通过醚化或酯化后,也适用本发明的目的。
这种化学改性可以在原料淀粉降解之前或之后进行。酯化不仅可以用无机酸,也可以用有机酸、其酐类或氯化物。其中最好的是磷酸盐化的和乙酰化了的衍生物。最广泛采用的醚化方法是在碱水溶液中用有机卤化物、环氧化物或硫酸盐进行处理。特别合适的醚类是烷基醚、羟烷基醚、羟烷基醚和烯丙基醚。也可以用氰烷基化衍生物,以及与2,3-环氧丙基三甲基铵氧化物的反应物。不过,没有经过化学改性的产物也是优选的。也可以用纤维素如纤维二糖和其低聚物的降解产物。
本发明特别适用的糖化淀粉是可工业化制得的产品(如C*PUR产品01906、01908、01910、01912、01915、01921、01924、01932或01934,生产厂为Cerestar)。这类糖化淀粉从化学上讲不同焙烧糊精,这是因为在水介质中有水解降解(一般为悬浮液或溶液,通常在固形物含量为10-30%(wt)、较好的是用酸或酶催化进行)时,根本没有再结合和支化的机会,其结果是不存在有不同分子量分布。例如,具有双峰分子量分布的糖化淀粉特别适合本发明的目的。制备糖化淀粉属于一般技术,可参见G.Tegge,Starke and Starkederivate,Behr′s Verlag,Hamburg1984,Page 173及220ff,也可参见EP-A-441197。
糖化淀粉在室温下可完全溶于水,溶解度极限一般为50%(wt)以上,这特别适合制备水聚合物分散液。
现已发现,糖化淀粉具有多分散度P为6-12的非常合适(按重均分子量Mw与数均分子量Mn的比值定义(用凝胶渗透色谱法可测量),p表示分子量分散)。
采用分子量1000以下的糖化淀粉重量比例为至少10%(wt)但不超过70%(wt)也是很好的。
也可采用右旋糖当量DE为5-40的糖化淀粉。DE值是指相对于无水右旋糖还原能力的还原能力,可以根据“食品及农产品专家委员会DIN 10308版5.71”(DIN 10308 Edition 5.71of the Specialist Committee on Foods and Agricultural Produets)进行测量(也可以参见Gunther Tegge,Starke und Starkederivate,Behr′s Verlag,Hamburg 1984,Page 305)。
现也发现,其特性分布特别好的含水聚合物分散液可用下列所说的糖化淀粉制得,强度为40%(wt),25℃下水溶液的动态粘度40[Pa.s]为0.005-0.06,较好为0.005-0.03,按DIN 53019测量,其剪切梯度为75s-1。
在自由基水乳化液聚合期间,糖化物不仅能够以各分散剂的形式存在,而且可以与其它表面活性物质混合。按所用单体的量计,于含水聚合物分散液中糖化物含量通常为1-50%(wt),较好为3-30%(wt)。
合适的附随表面活性物质原则上包括保护胶体和阴离子、阳离子或非离子型乳化剂,通常用作分散剂,合适的保护胶体的详细说明可参见“Houben-Weyl,Methoden der organischen Chemie,Volume ⅩⅠⅤ/1,Makromolekulare Stoppe,Georg.ThiemeVerlag,Stuttgart,1961,Pages 411-420”。附随的表面活性物质较好的是排他性的乳化剂,其分子量与保护胶体完全不同,通常在2000以下。当然,如果使用表面活性物质的混合物,各物质必须是彼此互溶的,这可以用预先小的试验来证实。所用的附随表面活性物质较好的为阴离子或非离子乳化剂。用户可选购的附随物质或共乳化剂包括如环氧化脂肪醇(环氧化(EO)值为3-50,烷基C8-C36)、环氧化一、二和三烷基酚(EO值为3-50,烷基C4-C9)、环氧化醇(EO值为4-30,烷基C12-C18)、环氧化烷基酚(EO值为3-50,烷基C4-C9)、磺酸琥珀酸之二烷基酯的碱金属盐,烷基硫酸盐(烷基C8-C12)、烷基磺酸(烷基C12-C18)、烷基二苯氧磺酸(烷基C12-C18)及烷基芳基磺酸(烷基C9-C18)的碱金属盐和铵盐以及相应的酸。在“Houben-Weyl,Methoden der organischen Chemie,Volume ⅩⅠⅤ/1,Makromolekulare Stoppe,Georg.Thieme Verlag,Stuttgart,1961,Pages 192-208”中介绍了另外一些合适的乳化剂。优选的是这样一些表面活性物质,即生物可降解的、无毒的、无毒降解的产品和二级产品,如十二烷基磺酸钠。按被聚合的单体的量计算,表面活性物质用量一般为0-5%(wt),较好为0.1-1%(wt)。
聚合温度一般为30-95℃,较好为75-90℃。聚合介质不仅可由水组成,也可由水溶性液体如甲醇组成。较好的是仅仅用水。乳化液聚合反应可在常规的带有混合元件的装置中进行,如搅拌烧瓶、锅、高压釜和圆形反应器。可以间歇式或连续式进行,如在阶式锅或其它内连聚合装置中进行。不仅可以采用间歇方法进行,也可以采用供料流增加法进行,包括阶段性或阶梯性的。优选的用供料流增加法,其中部分聚合物料作为起始原料供入,加热到聚合温度,聚合反应开始,接着加入剩余部分聚合物料,通常采用多次空间分隔流方式加入,其中一次或多次含有纯单体或乳化形单体,采用连续、分阶段或浓度梯度叠加方式进行,同时保持聚合反应区的聚合反应。从实用观点考虑,较好的是起始加料和/或单体流含有少量乳化剂,按被聚合的单体总量计,通常为0.5%(wt)以下,以便使分散介质的表面张力减小,因此,需要进行搅拌。因此,以后的单体就可以加入到用这些辅助乳化剂预乳化的聚合反应区内。较好的是,所用的所有糖化物在含水的起始加料中加入,通常以溶解形式加入。
合适的自由基聚合反应引发剂包括所有能够引发自由基含水乳化液聚合反应的物质,这些不仅是过氧化物,如碱金属过氧化硫酸盐、过氧化硫酸铵或H2O2,也可以是偶氮化合物。
也可以用由至少一种有机还原剂和至少一种过氧化物和/或过氧化氢组成的混合引发剂,例如,叔丁基氢过氧化物和羟甲烷磺酸或过氧化氢和抗坏血酸。也可以用混合系统,除了含有少量可溶于聚合介质中的金属化合物,其中的金属以高于一价的状态存在,例如,抗坏血酸/硫酸铁(Ⅱ)/过氧化氢混合系,尽管有抗坏血酸存在时,通常采用羧甲烷磺酸钠盐、亚硫酸钠、亚硫酸氢钠或焦亚硫酸钠,除了过氧化氢以外,通常可采用叔丁基氢过氧化物或碱金属过氧化二硫酸盐和/或过氧化二硫酸铵。一般地讲,基于被聚合的单体总量计,所用能自由基引发剂的量为0.1-2%(wt)。特别优选的是用过氧化硫酸氢铵和/或碱金属过氧化硫酸氢盐本身,或作为引发剂混合系的一部分。
当需要时,可以在有调节剂存在下进行自由基含水接枝聚合反应。合适的调节剂包括例如巯基化合物,象巯基乙醇、巯基丙醇、巯基丁醇、巯基乙酸、巯基丙酸、丁基巯醇和十二烷基巯醇。其它合适的调节剂是烷基化合物,如烷基醇。当在有调节剂存在下进行接枝聚合反应时,按聚合时所用单体量计,调节剂用量为0.05-20%(wt)。
当然,本发明的自由基含水聚合反应也可以在超临界压力或减压下进行。
一般来讲,制备的含水聚合物分散液的固体总含量为15-65%(wt),较好的为30-60%(wt)。
聚合物分散液可以与常规添加剂混合,一般情况下,在聚合反应结束后加入添加剂。合适的添加剂是交联非聚合物质,其含量通常为0.1-5%(wt)。当聚合物含有自由羧基时,就可以用能够交联该基团的化合物,如多价金属碱化合物,象氧化锌、氧化钙或相应的氢氧化物、乙酸盐或碳酸盐或相应的混合盐。也可以用可交联任何羟基的化合物,如二和多官能无机酸和酸衍生物,象磷酰氯、碱金属三甲基磷酸盐、碱金属多磷酸盐或碱金属四硼酸盐、二和多官能有机酸如己二酸、柠檬酸、1,2,3,4-丁烷四甲酸、全顺-1,2,3,4-环戊烷四甲酸、二和多官能有机酸的衍生物如酐或混合酐、象二乙酰基己二酸酐、乙酰柠檬酸酐、酰基氯如氰尿酰氯、咪唑烷(imidaxolides)和胍衍生物、也可以是二和多官能异氰酸如1,6-己二异氰酸酯、2,4-二异氰酸甲苯、二和多官能烷基化剂如表氯醇、二氯乙醚、双环氧化合物、各种醛类或醛衍生物如甲醛、乙醛、丙烯醛、2,5-二甲氧基甲氢呋喃或戊二醛(glutardialedhyde)。也可以采用基于甲醛、乙二醛、蜜胺、苯酚和/或尿素的浓缩产品。甲醛和含甲醛的交联剂系不太合适,因为有毒性残留物。
作为无纺织物的添加剂可以按已知量加入,生物可降解的物质为优选的。为保证产品特性,较好的是无纺织物中不含粘土或白垩。
按已知方法用聚合物将纤维网固结(如Ullmann′s Encyklopadie der technischen Chemie,4th Edition,Volume 23,1983,pages 738-742)。通常用聚合物分散液进行浴浸渍、泡沫浸渍、喷雾、轧染或印染使纤维网饱和。因为这种分散液可以用水稀释或用常规增稠剂增稠,以获得所需的加工粘度。用分散液处理纤维网后,一般要对生成的结合好的纤维网无纺织物进行干燥和加热处理。干燥条件取决于所用干燥器的特性,干燥温度一般为100-230℃,干燥和/或加热处理时间为10秒-60分钟。
本发明的无纺织物具有良好的堆肥性和优良的操作性能。其中包括干强度、湿强度和柔软手感。该产品的湿强度特别突出,因为糖化物是亲水物质,因此,湿强度完全是令人惊奇的。因低聚糖和多糖是已知的硬物质,这是由于多个氢键所致,所以本发明的无纺织物的柔软特性同样是令人惊奇的。
实施例
所用多糖是选自Cerestar Deutschland GmbH,D-1150 Krepeld 12的淀粉C*PUR 01915或01934。它们都有重要的双峰分子量分布,其特征如下:
型号 Mw U %(wt) DE 40
<1000 [Pa.s]
01915 6680-8350 6.8-8.4 32.9-34.7 17-19 0.021
01934 3000 6.0 68.4 36-39 0.009
用蒸汽压渗透法测量Mn,01915的值为980克/摩尔。
用传统方式凝胶渗透色谱法测量Mw和P,参数如下:
柱:3个包有TSK凝胶G2000PW、G3000PW和G4000PW的7.5 600mm钢柱,孔径为5μm
流动相:蒸馏水
温度:RT(室温)
检测:差示折光计(如ERC 7511)
流速:0.8ml/min.泵:(如ERC 64.00)
注射量:20μl阀:(如VICI 6通阀)
评定:Brucker Chromstar GPC软件
校准:在低分子量区用葡萄糖、棉子糖、麦芽糖和麦芽戊糖;在高分子量区用多分散性<1.2的支链淀粉标准物。
实施例1
将766g水、100g淀粉01915(选自Cerestar)和基于烷基二苯氧化磺酸(选自Dow的Dowfax 2Al)的商用乳化剂2.2g之混合物加热到85℃,与20%(wt)的料流2混合,5分钟后与10%(wt)料流1混合。在85℃下起始聚合反应15分钟后开始计量加入料流1和2的剩余部分。加入连续进行2.5小时(料流1)以上及3小时(料流2)以上。随后于85℃下进行后聚合1小时,冷却并加入内温度<30℃的2.9g叔丁基氢过氧化物(于水中70%(wt)浓度)。5分钟后,在超过15分钟时间里,将羟甲烷磺酸钠盐2g、硫酸铁(Ⅱ)铵0.1g、乙二胺四乙酸钠盐0.5g和水10g的混合物加入,随后搅拌30分钟。
根据DIN 53189测量,含水聚合物分散液的固形物含量约为44%(wt)。
由聚合物分散液形成的膜之玻璃化温度为-42℃(膜厚:0.5mm,干燥:于室温下30小时)。
料流1:
水 380g
丙烯酸正丁酯 950g
丙烯酸 20g
丙烯基酰胺乙醇酸 30g
Dowfax 2Al(于水中为45%浓度(wt) 2.2g
料流2:
过氧化硫酸氢钠 6g
水 200g
实施例2
将水365g、淀粉01915型35g的混合物加热到85℃,与20%(wt)料流2混合,5分钟后与10%(wt)料流1混合。在85℃下经起始聚合反应15分钟后,开始计量加入料流1和2的剩余部分。连续加入时间超过2.5小时(料流1)和3小时(料流2)。随后于85℃下进行后聚合1小时,冷却并加入内温度为70℃的1.4g叔丁基过氧化物(于水中为70%(wt)浓度)。5分钟后,在超过60分钟的时间里,加入羧甲烷磺酸钠盐1g、硫酸铁(Ⅱ)铵0.05g、乙二胺四乙酸钠盐0.25g和水5g的混合物,接着冷却至室温。
含水聚合物分散液的固形物含量为约44%(wt)。
玻璃化温度为-12℃(按实施例1所述方法测量)。
料流1:
水 190g
乙基丙烯酸酯 483g
丙烯基酰胺乙醇酸 17.5g
Dowfax 2Al(水中45%(wt)浓度) 5.6g
料流2:
过氧化硫酸氢钠 3g
水 100g
实施例3
将水882g、淀粉01915型63g和Dowfax 2Al 2.8g的混合物加热到85℃,与20%(wt)料流2混合,5分钟后与10%(wt)料流1混合,于85℃下起始聚合反应15分钟后,开始计量加入料流1和2的剩余部分。接着在85℃下进行后聚合反应1小时,冷却并加入70℃的叔丁基氢过氧化物3.6g(水中为70%(wt)浓度)。5分钟后,在超过15分钟时间里加入羟甲烷磺酸钠盐2.5g、硫酸铁(Ⅱ)铵0.13g、乙二胺四乙酸钠盐0.63g和水12.5g的混合物,随后搅拌30分钟。
含水聚合物分散液的固形物含量为约44%(wt)。
玻璃化温度为-34℃(按实施例1所说方法测量)。
料流1:
水 475g
丙烯酸正丁酯 875g
乙基丙烯酸酯 300g
丙烯酸 25g
丙烯基酰胺乙醇酸 50g
Dowfax 2Al(水中为45%(wt)浓度) 14g
料流2:
过氧化硫酸氢钠 7.5g
水 250g
实施例4
将水383g、淀粉01934型50g、Dowfax 2Al 1.11g的混合物加热到85℃,与20%(wt)料流2混合,5分钟后与10%(wt)料流1混合。于85℃下起始聚合反应15分钟后,开始计量加入料流1和2的剩余部分。连续加入时间超过2.5小时(料流1)和3小时(料流2)。接着于85℃下进行后聚合反应1小时,冷却并加入70℃的叔丁基氢过氧化物1.4g(水中为70%(wt)浓度)。5分钟后在超过15分钟时间里加入羟甲烷磺酸钠盐1g、硫酸铁(Ⅱ)铵0.05g、乙二胺四乙酸钠盐0.25g和水5g的混合物,接着搅拌30分钟。
含水聚合物分散液的固形物含量为约44%(wt)。
玻璃化温度为-11℃(按实施例1所说的测量)。
料流1:
水 190g
乙基丙烯酸酯 483g
丙烯基酰胺乙醇酸 17.5g
Dowfax 2Al(水中为45%(wt)浓度) 5.6g
料流2:
过氧化硫酸氢钠 3g
水 100g
实施例5
将水826g、乙酸钠2.5g和淀粉01934型62.5g的混合物加热到85℃,加入20%料流3和36%料流1。接着于85℃下进行起始聚合反应15分钟,再在超过1小时的时间里计量加入料流1的剩余部分和27%料流3。在料流1的加入结束时,在超过1.5小时的时间里加入料流2和在超过2小时的时间里加入料流3的其余部分。随后在85℃下进行起始聚合反应1小时,冷却至70℃并加入过氧化氢8.3g(于水中为30%浓度)。5分钟后,在超过1小时的时间内加入抗坏血酸2.5g、硫酸铁(Ⅱ)铵0.08g和水13g的混合物,将混合物搅拌30分钟,冷却至室温。
含水聚合物分散液的总固形物含量约为43%。
玻璃化温度为0℃。
料流1:
水 140g
乙基丙烯酸酯 338g
丙烯酰胺乙醇酸 12g
Steinapol NLS(水中15%浓度) 12g
料流2:
水 360g
乙基丙烯酸酯 287g
乙烯基丙酸酯 581g
丙烯酰胺乙醇酸 32g
Steinapol NLS(水中15%浓度) 30g
料流3:
过氧化硫酸氢钠 7.5g
水 250g
[Steinapol NLS=十二烷基磺酸钠]
实施例6
将水644g作为原料加入,加热到85℃,与20%料流2和10%料流1混合,接着于85℃下进行起始聚合反应15分钟,然后开始计量加入料流1和2的其余部分。加料连续进行2.5小时以上(料流1)和3小时以上(料流2)。再于85℃下进行后聚合反应1小时,冷却到70℃,加入叔丁基氢过氧化物2.9g(水中70%浓度)。5分钟后加入羟甲烷磺酸钠盐2g、硫酸铁(Ⅱ)铵0.1g、乙二胺四乙酸钠盐0.5g和水10g的混合物,加入时间超过1小时,随后搅拌混合物30分钟,冷却至室温。
含水聚合物分散液的固形物含量约为45%。
玻璃化温度为-11℃。
料流1:
水 380g
乙基丙烯酸酯 965g
丙烯酰胺乙醇酸 35g
Dowfax 2Al(水中45%浓度) 11.1g
C8-C10葡糖苷(水中55%浓度)
料流2:
过氧化硫酸氢钠 6g
水 200g
所用的C8-C10葡糖苷按DE-P4212080.2所述的下列方法进行制备:
向备有挡板、盘式搅拌器、测温计、蒸馏头、带有计量泵的计量装置、压力控制阀和喷嘴的2-1多颈搅拌反应器中装入663g表面活性剂C8-C10Spegial(Henkel,辛醇与癸醇的混合物),接着加入2.6g(0.008mol)十二烷基苯磺酸。将该混合物与121.6g烷基葡糖苷/醇乳化剂混合物(组成:63%表面活性剂、22.6%C12-二葡糖苷、2.2%C12-C12单葡糖苷、5.2%C12-四葡糖苷、<0.5%C12-五葡糖苷和5.9%多葡糖)。按所用葡萄糖计,乳化剂的含葡萄糖部分为30%。脂肪醇与葡萄糖的摩尔比为6∶1。
将溶液加热到115-120℃,于减压即30-35毫巴采用如下方式计量加入214g(0.83摩尔)的60℃右旋糖浆(70%浓度溶液,葡萄糖含量约99.5%),制备出根本不含有葡萄糖的特殊沉淀的浑浊乳液。计量加入4小时和搅拌30分钟后,蒸馏掉83g水,余下微浑浊的淡黄色反应溶液。
冷却至90℃后,用1.6g的50%浓度氢氧化钠溶液使催化剂失去活性,生成的溶液具有PH8.3(于50%浓度水溶液中测量)。于1毫巴真空下用薄膜蒸发器(加热温度170℃,流出温度140℃)除去多余醇。产品用水处理直接变成水溶液并于80℃下用12.3g H2O2(30%浓度溶液)进行漂白。
实施例7
将水661g作为原料加入,加热至85℃与20%料流2和10%料流1混合,接着于85℃下进行起始聚合反应15分钟,再开始计量加入料流1和2的其余部分。加入料流连续进行2.5小时以上(料流1)和3小时(料流2)以上。随后于85℃下进行后聚合反应1小时,冷却到70℃加入叔丁基氢过氧化物(于水中70%浓度)。5分钟后,在超过1小时的时间里加入2g羟甲烷磺酸钠盐、0.1g硫酸铁(Ⅱ)铵、0.5g乙二胺四乙酸钠盐和10g水的混合物,接着将混合物搅拌30分钟,冷却至室温。
含水聚合物分散液的固形物含量约为44%。
玻璃化温度为-11℃。
料流1:
水 380g
乙基丙烯酸酯 965g
丙烯酰胺乙醇酸 35g
Dowfax 2Al(水中45%浓度) 11.1g
C10-C12葡糖苷(水中47%浓度) 95g
料流2:
过氧化硫酸氢钠 6g
水 200g
所用C10-C12葡糖苷按实施例6所述方法制得,不同的是用754g Nafol 1012(选自Condea,为癸醇、十二烷醇和少量十四烷醇的混合物。
比较例1
在2升备有马蹄式搅拌器、用于单体、引发剂溶液和氨的加料装置、回流冷凝器及氮入口和出口的玻璃装置中,于20℃在氮气氛下将120g酪蛋白(酸型)悬浮于500g水,接一次性加入180g正丁基丙烯酸酯,于20℃下搅拌混合物15分钟,再在超过15分钟时间里滴加9g 25%浓度氨水溶液,滴加完后,于20℃下再搅拌混合物40分钟,再一次性加入20g的13%(wt)浓度的过氧化硫酸钠溶液,反应混合物的温度升至75℃。
当达到75℃时,在超过2小时的时间里,加入20g的10%浓度(wt)过氧化硫酸钠溶液,随后于70℃下将反应混合物再搅拌2小时,再加入1g叔丁基过新戊酸酯,于75℃下再搅拌混合物2小时。
比较例2
在聚合反应结束后加入淀粉重复进行实施例4。
比较例3
所用淀粉混合物是基于苯乙烯/丁二烯的乳液聚合物,制备过程不含糖化物,具有玻璃化温度为-16℃。
比较例4
将832水和2.8g Dowfax 2Al的混合物加热到85℃,与20%料流2和10%料流1混合,于85℃下进行起始聚合反应15分钟后,开始计量加入料流1和2的其余部分,料流连续加入时间超过2.5小时(料流1)和3小时(料流2),随后于85℃下进行后聚合1小时,冷却70℃,加入3.6g叔丁基氢过氧化物(于水中浓度为70%),5分钟后,加入2.5g羟甲烷磺酸钠盐、0.13g硫酸铁(Ⅱ)铵、0.63g乙二胺四乙酸钠盐和13g水的混合物,加过时间超过1小时,接着搅拌30分钟,冷却至室温。
含水聚合物分散液的总固形物含量约为44%。
料流1:
水 475g
丙烯酸丁酯 875g
丙烯酸乙酯 300g
羟乙基丙烯酸酯 50g
丙烯酸 25g
Dowfax 2Al(水中浓度45%) 14g
料流:
过氧化硫酸氢钠 7.5g
水 250g
向700份(wt)聚合物分散液中加入38.5份(wt)1,3-二甲基-4,5-二羟基咪唑啉-2-酮(水中浓度40%)溶液和31份柠檬酸(水中25%浓度)溶液的混合物,搅拌5分钟。
制备无纺织物:
将定量为35g/m2的纵向取向(纤维取向较好的为一个方向,纵向方向)的纤维素纤维网分次用上述实施例和比较例所这的分散液进行浸渍,首先稀释成均匀固形物含量为10%,经过两个逆向转动的辊以除去过量的分散液,接着暴露于150℃下4分钟,这样获得的无纺织物的粘合剂含量在所有情况下为25%(wt)。
分析无纺织物:
将无纺织物切成50mm宽的条,于干燥和水湿状态下模拟DIN 53857,采用自由挟持长度10cm,对这些条进行拉伸试验,以测量与优选纤维方向相切的断裂强度(通过适当切断试件)。
另外,将无纺织物试件绕金属心轴卷绕,以测量弯曲硬度,用以测量柔软度,弯曲硬度是一种必须具有的用以获得弯曲的力,与优选的纤维方向相切测量该力。
这些试验的结果列入表1。
表1
实施例与比较例 拉伸强度[N] 弯曲硬度[mN]
干 水湿
实施例1 33 8 24
实施例2 34 9 41
实施例3 31 13 21
实施例4 33 8 24
实施例5 13
实施例6 13
实施例7 11
比较例1 91 <1 130
比较例2 12 20
比较例3 47 13 30
比较例4 10 6 20
为测试本发明获得之无纺织物的堆肥性能,与DIN 53933掩埋试验相同,对无纺织物进行掩埋试验,即埋入密封堆肥池中,放置限定时间。将无纺织物挖出后,对其进行断裂强度测试,与没有掩埋的相应样品的断裂强度进行比较,以测量因堆肥掩埋造成的断裂强度损失。这种断裂强度的损失用以测量堆肥性。另外,用目测无纺织物试件的分解度。断裂强度损失越高,试件的目测分解度越大,无纺织物的堆肥性越好。
按上述方法制备用于堆肥试验的无纺织物,但所用的原料网是定量为50g/m2的轻度预针刺的粘胶纤维网。堆肥试验的结果列入表2。
表2
实施例 掩埋前断裂强度(干) 掩埋后断裂强度(干)9天
实施例1 27N 5N
实施例3 25N 13N
比较例3 40N 30N
无固结原料网 10N 2N
无纺织物试件的目测结果说明,按比较例3粘合的试件经掩埋后无任何可见的分解显示。与之相反,用实施例1和3粘合的无纺织物,具有很明显的分解特征,即试件明显变薄,并且有老化的小孔。
Claims (8)
1、一种无纺织物,按所用纤维重量计,粘合有5-100%(wt)的玻璃化温度为-70-40℃的聚合物,该聚合物是在有糖化物存在下的水介质中通过烯键不饱和单体混合物的自由基聚合反应制备的,单体混合物含有0.5-15%(wt)单烯键不饱和C3-C10羧酸、丙烯酰胺乙醇酸、甲丙烯酰胺乙醇酸的N-醇酰胺、或其醚类、酯类或与碳原子达12之醇类形成的醚-酯类。
2、根据权利要求1的无纺织物,其中糖化物具有重均分子量1000-25000。
3、根据权利要求1的无纺织物,其中所用糖化物是糊精。
4、根据权利要求1的无纺织物,其中所用糖化物是用水相水解法获得的淀粉降解产物。
5、根据权利要求1的无纺织物,其中所用糖化物是单糖或低聚糖与具有6-18个碳原子醇类形成的乙缩醛。
6、根据权利要求1的无纺织物,其中的聚合物含有:
70-99.5%(wt)丙烯酸和/或甲基丙烯酸与含有1-12个碳原子之醇形成的酯类、苯乙烯、丁二烯、乙烯基乙酸酯和/或丙酸酯,
0.5-15%(wt)单烯键不饱和的3-10个碳原子的羧酸、丙烯酰胺乙醇酸、甲丙烯酰胺乙醇酸的N-醇酰胺、其与具有达12个碳原子之醇形成的醚、酯或醚-酯,
0-15%(wt)其它单体。
7、固结纤维网的方法,包括按所用纤维重量计用5-100%(wt)玻璃化温度为-70-40℃的聚合物,该聚合物采用在有糖化物存在下的水介质中对烯键不饱和单体的混合物进行自由基聚合反应进行制备,单体混合物包括0.5-15%(wt)单烯键不饱和的具有3-10个碳原子羧酸、丙烯酰胺乙醇酸、甲基丙烯酰胺乙醇酸的N-醇酰胺、其具有达12个碳原子的醚、酯或醚-酯。
8、用权利要求1的无纺织物加工尿布的方法。
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DE10342858A1 (de) * | 2003-09-15 | 2005-04-21 | Basf Ag | Verwendung formaldehydfreier wässriger Bindemittel für Substrate |
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DE59305131D1 (de) | 1997-02-27 |
FI934386A0 (fi) | 1993-10-06 |
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