CN101677575A - 抗微生物塑料及涂料 - Google Patents
抗微生物塑料及涂料 Download PDFInfo
- Publication number
- CN101677575A CN101677575A CN200880016472A CN200880016472A CN101677575A CN 101677575 A CN101677575 A CN 101677575A CN 200880016472 A CN200880016472 A CN 200880016472A CN 200880016472 A CN200880016472 A CN 200880016472A CN 101677575 A CN101677575 A CN 101677575A
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- CN
- China
- Prior art keywords
- silver
- coating
- polymer
- butyl
- carrier
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 106
- 229910052709 silver Inorganic materials 0.000 claims abstract description 106
- 239000004332 silver Substances 0.000 claims abstract description 106
- 239000000203 mixture Substances 0.000 claims abstract description 67
- 229920000642 polymer Polymers 0.000 claims abstract description 65
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims abstract description 33
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- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 description 1
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- 238000010998 test method Methods 0.000 description 1
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- 239000004308 thiabendazole Substances 0.000 description 1
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- WJCNZQLZVWNLKY-UHFFFAOYSA-N thiabendazole Chemical compound S1C=NC(C=2NC3=CC=CC=C3N=2)=C1 WJCNZQLZVWNLKY-UHFFFAOYSA-N 0.000 description 1
- 229960004546 thiabendazole Drugs 0.000 description 1
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- XFNJVJPLKCPIBV-UHFFFAOYSA-N trimethylenediamine Chemical class NCCCN XFNJVJPLKCPIBV-UHFFFAOYSA-N 0.000 description 1
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- 150000003672 ureas Chemical class 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
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- 150000003751 zinc Chemical class 0.000 description 1
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- PICXIOQBANWBIZ-UHFFFAOYSA-N zinc;1-oxidopyridine-2-thione Chemical compound [Zn+2].[O-]N1C=CC=CC1=S.[O-]N1C=CC=CC1=S PICXIOQBANWBIZ-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/83—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/14—Paints containing biocides, e.g. fungicides, insecticides or pesticides
Abstract
通过向其中掺入元素银和负载于沸石或玻璃上的银,该塑料和涂料被赋予突出的抗微生物活性。该组合物适用于医疗用途,例如管(tubes)、导管(catheters)、织物等等。该塑料织物为纺织的或无纺的。该塑料为例如聚氨酯、聚碳酸脂、液体硅橡胶、聚丙烯或聚乙烯或高分子复合材料。
Description
本发明的涉及抗微生物聚合物及涂料组合物,例如用于医药用途的组合物。通过掺入元素银和负载于沸石或玻璃上的银的组合,所述聚合物及涂料被赋予突出的抗微生物活性。
背景技术
美国专利第4,775,585、4,911,898、4,911,899和6,071,542号公开了带有沸石载体的银。
美国专利第6,585,989号也教导了带有沸石载体的银。
例如在已公布美国申请第2005/0233888号公开了带有玻璃载体的银。
例如在已公布的美国申请第2006/0134313号教导了抗菌塑料制品。美国专利第6,822,034号教导了抗微生物硅橡胶。美国专利第6,984,392号教导了抗微生物金属银。美国专利第5,049,139号公开了一些医疗器械,其包含由浸银玻璃组成的设计用于流体接触的部分。美国专利第5,730,995号公开了一些抗菌胶体,其包括某种无机氧化物和银。
令人惊讶的是,掺入元素银和负载于沸石或玻璃上的银的组合的聚合物或涂料显示较好的抗微生物效果。
概述
公开了抗微生物聚合物或涂料,所述聚合物或涂料包括有效抗微生物量的元素银和带有载体的银,所述带有载体的银负载于沸石或玻璃上。
也公开了赋予聚合物或涂料以抗微生物活性的方法,该方法包括向其中掺入有效抗微生物量的元素银和带有载体的银,其中所述带有载体的银负载于沸石或玻璃上。
详细说明
例如美国专利第4,775,585、4,911,898、4,911,899、6,071,542或6,585,989号中教导了带有沸石载体的银,其相关公开内容通过引用并入本文。
沸石通常是具有三维生长的骨架结构的铝硅酸盐,并通常用xM2/nO·Al2O3·ySiO2·zH2O表示,以Al2O3作为基础,其中M表示可离子交换金属离子,其通常是单价或二价金属离子;n对应所述金属的价态;x是所述金属氧化物的系数;y是二氧化硅的系数;以及z是结晶水的数值。本发明的沸石具有至少150m2/g的比表面积。所述沸石负载着抗微生物银,也就是说,银保留在所述沸石的可离子交换部位。
根据美国专利第6,071,542号,所述带有沸石载体的银可以是由沸石负载的表面改性的银。
所述带有玻璃载体的银也可以包括锌,即可以是银玻璃或银锌玻璃。例如在已公布的美国申请第2005/0233888号中教导了带有玻璃载体的银,其公开内容通过引用并入本文。
基于银和载体材料的总重,负载于沸石或玻璃上的银代表性地包含大约0.1到10%,特别是0.5到5%的银。带有载体的银颗粒通常是微米级,其平均粒度为例如大约1到100微米,特别是1到20微米。
所述元素银可以是微米级或纳米级。例如在美国专利第6,822,034号中公开了纳米级的抗菌银,其相关公开内容通过引用并入本文;这些纳米粒子的代表性粒度平均值为例如大约1到50nm不等,或大约10到1000nm,特别是10到100nm。该参考资料也教导了液体硅橡胶。美国专利第No.6,984,392号,特别见第2列第18-62行及第3列第3-20行,以及US-A-2006-018943中,教导了微米级多孔粒子形式的金属抗微生物银,其公开内容通过引用并入本文;这些微米粒子的代表性粒度平均值为大约1到20微米不等,优选10到20微米。
基于所述聚合物或涂料固体的重量,所述元素银的用量为例如大约0.01到大约5.0重量%。例如,基于所述聚合物或涂料固体的重量,所述元素银的用量为大约0.01到大约2.0重量%或大约0.01到大约1.0重量%。
基于所述聚合物或涂料固体的重量,所述带有载体的银的用量为例如大约0.001到大约0.2重量%。例如,基于所述聚合物或涂料固体的重量,所述带有载体的银的用量为大约0.01到大约0.2重量%或大约0.05到大约0.2重量%。这些重量含量以银为基础。
所述元素银/带有载体的银的重量/重量比(以银为基础)为例如大约10∶1到大约1000∶1,特别是大约10∶1到大约100∶1。
所述聚合物或涂料还可以进一步包含其它抗微生物剂,例如3,5-二甲基-四氢-1,3,5-2H-硫二嗪-2-硫酮、双-三丁基氧化锡、4.5-二氯-2-正辛基-4-异噻唑啉-3-酮、N-丁基-苯并异噻唑啉、10,10’-氧代双吩噁砒(10,10-oxybisphenoxarsine)、锌-2-吡啶硫醇-1-氧化物、2-甲基硫基-4-环丙氨基-6-(α,β-二甲基丙基氨基)-s-三嗪、2-甲基硫基-4-环丙氨基-6-叔丁氨基-s-三嗪、2-甲基硫基-4-乙氨基-6-(α,β-二甲基丙基氨基)-s-三嗪、2,4,4’-三氯-2’-羟基二苯醚、IPBC、多菌灵(carbendazim)或噻菌灵(thiabendazole)。
本发明的聚合物、聚合物组合物或涂料还可以包含一种或多种常规添加剂,如下列成分:
1.抗氧化剂
1.1.烷基化单酚,例如2,6-二叔丁基-4-甲基苯酚、2-叔丁基-4,6-二甲基苯酚、2,6-二叔丁基-4-乙基苯酚、2,6-二叔丁基-4-正丁基苯酚、2,6-二叔丁基-4-异丁基苯酚、2,6-二环戊基-4-甲基苯酚、2-(α-甲基环己基)-4,6-二甲基苯酚、2,6-双十八烷基-4-甲基苯酚、2,4,6-三环己基苯酚、2,6-二叔丁基-4-甲氧基甲基苯酚、侧链为直链或支化的壬基苯酚,例如2,6-二壬基-4-甲基苯酚、2,4-二甲基-6-(1’-甲基十一烷-1’-基)苯酚、2,4-二甲基-6-(1’-甲基十七烷-1’-基)苯酚、2,4-二甲基-6-(1’-甲基十三烷-1’-基)苯酚及其混合物。
1.2.烷基硫基甲基苯酚,例如2,4-二辛基硫基甲基-6-叔丁基苯酚、2,4-二辛基硫基甲基-6-甲基苯酚、2,4-二辛基硫基甲基-6-乙基苯酚、2,6-双十二烷基硫基甲基-4-壬基苯酚。
1.3.氢醌和烷基化氢醌,例如2,6-二叔丁基-4-甲氧基苯酚、2,5-二叔丁基氢醌、2,5-二叔戊基氢醌、2,6-二苯基-4-十八烷氧基苯酚、2,6-二叔丁基氢醌、2,5-二叔丁基-4-羟基苯甲醚、3,5-二叔丁基-4-羟基苯甲醚、3,5-二叔丁基-4-羟基苯基硬脂酸酯、双-(3,5-二叔丁基-4-羟基苯基)己二酸酯。
1.4.生育酚,例如α-生育酚、β-生育酚、γ-生育酚、δ-生育酚及其混合物(维生素E)。
1.5.羟基化硫代二苯醚,例如2,2’-硫代二(6-叔丁基-4-甲基苯酚)、2,2’-硫代二(4-辛基苯酚)、4,4’-硫代二(6-叔丁基-3-甲基苯酚)、4,4’-硫代二(6-叔丁基-2-甲基苯酚)、4,4’-硫代二(3,6-二仲戊基苯酚)、4,4’-二(2,6-二甲基-4-羟基苯基)二硫化物。
1.6.亚烷基双酚,例如2,2’-亚甲基双(6-叔丁基-4-甲基苯酚)、2,2’-亚甲基双(6-叔丁基-4-乙基苯酚)、2,2’-亚甲基双[4-甲基-6-(α-甲基环己基)苯酚]、2,2’-亚甲基双(4-甲基-6-环己基苯酚)、2,2’-亚甲基双(6-壬基-4-甲基苯酚)、2,2’-亚甲基双(4,6-二叔丁基苯酚)、2,2’-亚乙基双(4,6-二叔丁基苯酚)、2,2’-亚乙基双(6-叔丁基-4-异丁基苯酚)、2,2’-亚甲基双[6-(α-甲基苄基)-4-壬基苯酚]、2,2’-亚甲基双[6-(α,α-二甲基苄基)-4-壬基苯酚]、4,4’-亚甲基双(2,6-二叔丁基苯酚)、4,4’-亚甲基双(6-叔丁基-2-甲基苯酚)、1,1-双(5-叔丁基-4-羟基-2-甲基苯基)丁烷、2,6-双(3-叔丁基-5-甲基-2-羟基苄基)-4-甲基苯酚、1,1,3-三(5-叔丁基-4-羟基-2-甲基苯基)丁烷、1,1-双(5-叔丁基-4-羟基-2-甲基-苯基)-3-正十二烷基巯基丁烷、乙二醇双[3,3-二(3’-叔丁基-4’-羟基苯基)丁酸酯]、双(3-叔丁基-4-羟基-5-甲基-苯基)二环戊二烯、双[2-(3’-叔丁基-2’-羟基-5’-甲基苄基)-6-叔丁基-4-甲基苯基]对苯二酸酯、1,1-二-(3,5-二甲基-2-羟基苯基)丁烷、2,2-二(3,5-二叔丁基-4-羟基苯基)丙烷、2,2-二(5-叔丁基-4-羟基-2-甲基苯基)-4-正十二烷基巯基丁烷、1,1,5,5-四-(5-叔丁基-4-羟基-2-甲基苯基)戊烷。
1.7.O-、N-和S-苄基化合物,例如3,5,3’,5’-四叔丁基-4,4’-二羟基二苄基醚、4-羟基-3,5-二甲基苄基巯基乙酸十八烷基酯、4-羟基-3,5-二叔丁基苄基巯基乙酸十三烷基酯、三(3,5-二叔丁基-4-羟基苄基)胺、双(4-叔丁基-3-羟基-2,6-二甲基苄基)二硫代对苯二甲酸酯、双(3,5-二叔丁基-4-羟基苄基)硫醚、3,5-二叔丁基-4-羟基苄基巯基乙酸异辛基酯。
1.8.羟基苄基化丙二酸酯,例如2,2-二(3,5-二叔丁基-2-羟基苄基)丙二酸双十八烷基酯、2-(3-叔丁基-4-羟基-5-甲基苄基)丙二酸双十八烷基酯、2,2-二(3,5-二叔丁基-4-羟基苄基)丙二酸双十八烷基巯基乙基酯、2,2-二(3,5-二叔丁基-4-羟基苄基)丙二酸双[4-(1,1,3,3-四甲基丁基)苯基]酯。
1.9.芳香族羟基苄基化合物,例如1,3,5-三(3,5-二叔丁基-4-羟基苄基)-2,4,6-三甲基苯、1,4-二(3,5-二叔丁基-4-羟基苄基)-2,3,5,6-四甲基苯、2,4,6-三(3,5-二叔丁基-4-羟基苄基)苯酚。
1.10.三嗪化合物,例如2,4-二辛基巯基-6-(3,5-二叔丁基-4-羟基-苯胺基)-1,3,5-三嗪、2-辛基巯基-4,6-二(3,5-二叔丁基-4-羟基苯胺基)-1,3,5-三嗪、2-辛基巯基-4,6-二(3,5-二叔丁基-4-羟基苯氧基)-1,3,5-三嗪、2,4,6-三(3,5-二叔丁基-4-羟基苯氧基)-1,2,3-三嗪、1,3,5-三(3,5-二叔丁基-4-羟基苄基)异氰尿酸酯、1,3,5-三(4-叔丁基-3-羟基-2,6-二甲基苄基)异氰尿酸酯、2,4,6-三-(3,5-二叔丁基-4-羟基苯乙基)-1,3,5-三嗪、1,3,5-三(3,5-二叔丁基-4-羟基苯丙酰基)-六氢-1,3,5-三嗪、1,3,5-三(3,5-二环己基-4-羟基苄基)异氰尿酸酯。
1.11.苄基膦酸酯,例如2,5-二叔丁基-4-羟基苄基膦酸二甲酯、3,5-二叔丁基-4-羟基苄基膦酸二乙酯、3,5-二叔丁基-4-羟基苄基膦酸双十八烷基酯、5-叔丁基-4-羟基-3-甲基苄基膦酸双十八烷基酯、3,5-二叔丁基-4-羟基苄基膦酸单乙酯的钙盐。
1.12.酰氨基酚,例如4-羟基月桂酰苯胺、4-羟基硬脂酰苯胺、N-(3,5-二叔丁基-4-羟基苯基)氨基甲酸辛酯。
1.13.β-(3,5-二叔丁基-4-羟基苯基)丙酸与一元或多元醇形成的酯,所述一元或多元醇例如甲醇、乙醇、正辛醇、异辛醇、十八醇、1,6-己二醇、1,9-壬二醇、乙二醇、1,2-丙二醇、新戊二醇、硫代二乙二醇、二乙二醇、三乙二醇、季戊四醇、三羟乙基异氰尿酸酯、N,N’-二羟乙基草酰胺、3-硫代十一醇、3-硫代十五醇、三甲基己二醇、三羟甲基丙烷、4-羟甲基-1-磷-2,6,7-三氧二环[2.2.2]辛烷。
1.14.β-(5-叔丁基-4-羟基-3-甲苯基)丙酸与一元或多元醇形成的酯,所述一元或多元醇例如甲醇、乙醇、正辛醇、异辛醇、十八醇、1,6-己二醇、1,9-壬二醇、乙二醇、1,2-丙二醇、新戊二醇、硫代二乙二醇、二乙二醇、三乙二醇、季戊四醇、三羟乙基异氰尿酸酯、N,N’-二羟乙基草酰胺、3-硫代十一醇、3-硫代十五醇、三甲基己二醇、三羟甲基丙烷、4-羟甲基-1-磷-2,6,7-三氧二环[2.2.2]辛烷;3,9-二[2-{3-(3-叔丁基-4-羟基-5-甲基苯基)丙酰氧基}-1,1-二甲基乙基]-2,4,8,10-四氧杂螺[5.5]十一烷。
1.15.β-(3,5-二环己基-4-羟基苯基)丙酸与单元或多元醇形成的酯,所述一元或多元醇例如甲醇、乙醇、辛醇、十八醇、1,6-己二醇、1,9-壬二醇、乙二醇、1,2-丙二醇、新戊二醇、硫代二乙二醇、二乙二醇、三乙二醇、季戊四醇、三羟乙基异氰尿酸酯、N,N’-二羟乙基草酰胺、3-硫代十一醇、3-硫代十五醇、三甲基己二醇、三羟甲基丙烷、4-羟甲基-1-磷-2,6,7-三氧二环[2.2.2]辛烷。
1.16.3,5-二叔丁基-4-羟基苯基乙酸与一元或多元醇形成的酯,所述一元或多元醇例如甲醇、乙醇、辛醇、十八醇、1,6-己二醇、1,9-壬二醇、乙二醇、1,2-丙二醇、新戊二醇、硫代二乙二醇、二乙二醇、三乙二醇、季戊四醇、三羟乙基异氰尿酸酯、N,N’-二羟乙基草酰胺、3-硫代十一醇、3-硫代十五醇、三甲基己二醇、三羟甲基丙烷、4-羟甲基-1-磷-2,6,7-三氧二环[2.2.2]辛烷。
1.17.β-(3,5-二叔丁基-4-羟基苯基)丙酸的酰胺,例如N,N’-双(3,5-二叔丁基-4-羟基苯基丙酰基)六亚甲基二酰胺、N,N’-双(3,5-二叔丁基-4-羟基-苯基丙酰基)三亚甲基二酰胺、N,N’-双(3,5-二叔丁基-4-羟基苯基丙酰基)酰肼、N,N’-双[2-(3-[3,5-二叔丁基-4-羟基苯基]丙酰氧基)乙基]草酰胺(Nau-XL-1,由Uniroyal提供)。
1.18.抗坏血酸(维生素C)
1.19.胺类抗氧化剂,例如N,N’-二异丙基-对苯二胺、N,N’-二仲丁基-对苯二胺、N,N’-双(1,4-二甲基戊基)-对苯二胺、N,N’-双(1-乙基-3-甲基戊基)-对苯二胺、N,N’-双(1-甲基庚基)-对苯二胺、N,N’-二环己基-对苯二胺、N,N’-二苯基-对苯二胺、N,N’-双(2-萘基)-对苯二胺、N-异丙基-N’-苯基-对苯二胺、N-(1,3-二甲基丁基)-N’-苯基-对苯二胺、N-(1-甲基庚基)-N’-苯基-对苯二胺、N-环己基-N’-苯基-对苯二胺、4-(对甲苯氨磺酰)二苯基胺(4-(p-toluenesulfamoyl)diphenylamine)、N,N’-二甲基-N,N’-二仲丁基-对苯二胺、二苯基胺、N-烯丙基二苯基胺、4-异丙氧基二苯基胺、N-苯基-1-萘胺、N-(4-叔辛基苯基)-1-萘胺、N-苯基-2-萘胺、辛基化二苯基胺,例如对,对’-二叔辛基二苯基胺、4-正丁基氨基苯酚、4-丁酰氨基苯酚、4-壬酰氨基苯酚、4-十二烷酰氨基苯酚、4-十八烷酰氨基苯酚、双(4-甲氧基苯基)胺、2,6-二叔辛基-4-二甲基氨基甲基苯酚、2,4’-二氨基二苯基甲烷、4,4’-二氨基二苯基甲烷、N,N,N’,N’-四甲基-4,4’-二氨基二苯基甲烷、1,2-双[(2-甲基苯基)氨基]乙烷、1,2-二(苯基氨基)丙烷、(邻甲苯基)双胍、双[4-(1’,3’-二甲基丁基)苯基]胺、叔辛基化N-苯基-1-萘胺、单烷基化和二烷基化叔丁基/叔辛基二苯基胺的混合物、单烷基化和二烷基化壬基二苯基胺的混合物、单烷基化和二烷基化十二烷基二苯基胺的混合物、单烷基化和二烷基化异丙基/异己基二苯基胺的混合物、单烷基化和二烷基化叔丁基二苯基胺的混合物、2,3-二氢-3,3-二甲基-4H-1,4-苯并噻嗪、吩噻嗪、单烷基化和二烷基化叔丁基/叔辛基吩噻嗪的混合物、单烷基化和二烷基化叔辛基吩噻嗪的混合物、N-烯丙基吩噻嗪、N,N,N’,N’-四苯基-1,4-二氨基丁-2-烯。
2.紫外线吸收剂和光稳定剂
2.1.2-(2’-羟基苯基)苯并三唑,例如2-(2’-羟基-5’-甲基苯基)-苯并三唑、2-(3’,5’-二叔丁基-2’-羟基苯基)苯并三唑、2-(5’-叔丁基-2’-羟基苯基)苯并三唑、2-(2’-羟基-5’-(1,1,3,3-四甲基丁基)苯基)苯并三唑、2-(3’,5’-二叔丁基-2’-羟基苯基)-5-氯-苯并三唑、2-(3’-叔丁基-2’-羟基-5’-甲基苯基)-5-氯-苯并三唑、2-(3’-仲丁基-5’-叔丁基-2’-羟基苯基)苯并三唑、2-(2’-羟基-4’-辛氧基苯基)苯并三唑、2-(3’,5’-二叔戊基-2’-羟基苯基)苯并三唑、2-(3’,5’-双(α,α-二甲基苄基)-2’-羟基苯基)苯并三唑、2-(3’-叔丁基-2’-羟基-5’-(2-辛氧基羰基乙基)苯基)-5-氯-苯并三唑、2-(3’-叔丁基-5’-[2-(2-乙基己氧基)-羰基乙基]-2’-羟基苯基)-5-氯-苯并三唑、2-(3’-叔丁基-2’-羟基-5’-(2-甲氧基羰基乙基)苯基)-5-氯-苯并三唑、2-(3’-叔丁基-2’-羟基-5’-(2-甲氧基羰基乙基)苯基)苯并三唑、2-(3’-叔丁基-2’-羟基-5’-(2-辛氧基羰基乙基)苯基)苯并三唑、2-(3’-叔丁基-5’-[2-(2-乙基己氧基)羰基乙基]-2’-羟基苯基)苯并三唑、2-(3’-十二烷基-2’-羟基-5’-甲基苯基)苯并三唑、2-(3’-叔丁基-2’-羟基-5’-(2-异辛氧基羰基乙基)苯基苯并三唑、2,2’-亚甲基-双[4-(1,1,3,3-四甲基丁基)-6-苯并三唑-2-基酚];2-[3’-叔丁基-5’-(2-甲氧基羰基乙基)-2’-羟基苯基]-2H-苯并三唑与聚乙二醇300的酯交换产物;其中R=3’-叔丁基-4’-羟基-5’-2H-苯并三唑-2-基苯基、2-[2’-羟基-3’-(α,α-二甲基苄基)-5’-(1,1,3,3-四甲基丁基)-苯基]苯并三唑;2-[2’-羟基-3’-(1,1,3,3-四甲基丁基)-5’-(α,α-二甲基苄基)苯基]苯并三唑。
2.2.2-羟基二苯甲酮,例如其4-羟基、4-甲氧基、4-辛氧基、4-癸氧基、4-十二烷氧基、4-苄氧基、4,2’,4’-三羟基和2’-羟基-4,4’-二甲氧基衍生物。
2.3.取代和未取代苯甲酸酯,例如水杨酸-4-叔丁基苯酯、水杨酸苯酯、水杨酸-辛基苯酯、联苯甲酰基间苯二酚、双(4-叔丁基苯甲酰基)间苯二酚、苯甲酰基间苯二酚、3,5-二叔丁基-4-羟基苯甲酸-2,4-二叔丁基苯酯、3,5-二叔丁基-4-羟基苯甲酸十六烷基酯、3,5-二叔丁基-4-羟基苯甲酸十八烷基酯、3,5-二叔丁基-4-羟基苯甲酸-2-甲基-4,6-二叔丁基苯酯。
2.4.丙烯酸酯,例如α-氰基-β,β-二苯基丙烯酸乙酯、α-氰基-β,β-二苯基丙烯酸异辛酯、α-甲氧羰基肉桂酸甲酯、α-氰基-β-甲基-对甲氧基肉桂酸甲酯、α-氰基-β-甲基-对甲氧基-肉桂酸丁酯、α-甲氧羰基-对甲氧基肉桂酸甲酯、N-(β-甲氧羰基-β-氰基乙烯基)-2-甲基吲哚啉、四(α-氰基-β,β-二苯基丙烯酸新戊酯。
2.5.镍化合物,例如2,2’-硫代-双[4-(1,1,3,3-四甲基丁基)苯酚]的镍配合物,比如含有或不含有如正丁基胺、三乙醇胺或N-环己基二乙醇胺等其它配体的1∶1或1∶2的配合物、二丁基二硫代氨基甲酸镍、4-羟基-3,5-二叔丁基苄基膦酸的如甲基或乙基酯等单烷基酯的镍盐、酮肟如2-羟基-4-甲基苯基十一烷基酮肟的镍配合物、含有或不含有其它配体的1-苯基-4-月桂酰基-5-羟基吡唑的镍配合物。
2.6.立体受阻胺,例如双(2,2,6,6-四甲基-4-哌啶基)癸二酸酯、双(2,2,6,6-四甲基-4-哌啶基)琥珀酸酯、双(1,2,2,6,6-五甲基-4-哌啶基)癸二酸酯、双(1-辛氧基-2,2,6,6-四甲基-4-哌啶基)癸二酸酯、正丁基-3,5-二叔丁基-4-羟基苄基丙二酸-双(1,2,2,6,6-五甲基-4-哌啶基)酯,1-(2-羟乙基)-2,2,6,6-四甲基-4-羟基哌啶和琥珀酸的缩合物、N,N’-双(2,2,6,6-四甲基-4-哌啶基)六亚甲基二胺和4-叔辛基氨基-2,6-二氯-1,3,5-三嗪的直链或环状缩合物、三(2,2,6,6-四甲基-4-哌啶基)次氮基三乙酸酯、四(2,2,6,6-四甲基-4-哌啶基)-1,2,3,4-丁烷四羧酸酯、1,1’-(1,2-乙二基)-双(3,3,5,5-四甲基哌嗪酮),4-苯甲酰基-2,2,6,6-四甲基哌啶、4-硬脂酰氧基-2,2,6,6-四甲基哌啶、双(1,2,2,6,6-五甲基哌啶基)-2-正丁基-2-(2-羟基-3,5-二叔丁基苄基)丙二酸酯、3-正辛基-7,7,9,9-四甲基-1,3,8-三氮杂螺[4.5]癸烷-2,4-二酮、双(1-辛氧基-2,2,6,6-四甲基哌啶基)癸二酸酯、双(1-辛氧基-2,2,6,6-四甲基哌啶基)琥珀酸酯、N,N’-双(2,2,6,6-四甲基-4-哌啶基)六亚甲基二胺和4-吗啉基-2,6-二氯-1,3,5-三嗪的直链或环状缩合物、2-氯-4,6-二(4-正丁基氨基-2,2,6,6-四甲基哌啶基)-1,3,5-三嗪和1,2-二(3-氨基丙氨基)乙烷的缩合物、2-氯-4,6-二-(4-正丁基氨基-1,2,2,6,6-五甲基哌啶基)-1,3,5-三嗪和1,2-二(3-氨基丙氨基)乙烷的缩合物、8-乙酰基-3-十二烷基-7,7,9,9-四甲基-1,3,8-三氮杂螺[4.5]癸烷-2,4-二酮、3-十二烷基-1-(2,2,6,6-四甲基-4-哌啶基)吡咯烷-2,5-二酮、3-十二烷基-1-(1,2,2,6,6-五甲基-4-哌啶基)吡咯烷-2,5-二酮、4-十六烷氧基-和4-硬脂酰氧基-2,2,6,6-四甲基哌啶的混合物、N,N’-双(2,2,6,6-四甲基-4-哌啶基)六亚甲基二胺和4-环己基氨基-2,6-二氯-1,3,5-三嗪的缩合物、1,2-二(3-氨基丙氨基)乙烷和2,4,6-三氯-1,3,5-三嗪以及4-丁基氨基-2,2,6,6-四甲基哌啶的缩合物(CAS登记号[136504-96-6]);1,6-己二胺和2,4,6-三氯-1,3,5-三嗪以及N,N-二丁基胺和4-丁基氨基-2,2,6,6-四甲基哌啶的缩合物(CAS登记号[192268-64-7]);N-(2,2,6,6-四甲基-4-哌啶基)-正十二烷基琥珀酰亚胺、N-(1,2,2,6,6-五甲基-4-哌啶基)-正十二烷基琥珀酰亚胺、2-十一烷基-7,7,9,9-四甲基-1-氧杂-3,8-二氮杂-4-氧代-螺[4,5]癸烷(2-undecyl-7,7,9,9-tetramethyl-1-oxa-3,8-diaza-4-oxo-spiro[4,5]decane)、7,7,9,9-四甲基-2-环十一烷基-1-氧杂-3,8-二氮杂-4-氧代螺-[4,5]癸烷(7,7,9,9-tetramethyl-2-cycloundecyl-1-oxa-3,8-diaza-4-oxospiro[4,5]decane)和表氯醇的反应产物、1,1-二(1,2,2,6,6-五甲基-4-哌啶氧羰基)-2-(4-甲氧基苯基)乙烯、N,N’-二甲酰基-N,N’-双(2,2,6,6-四甲基-4-哌啶基)六亚甲基二胺、4-甲氧基亚甲基丙二酸与1,2,2,6,6-五甲基-4-羟基哌啶形成的二酯、聚[甲基丙基-3-氧-4-(2,2,6,6-四甲基-4-哌啶基)]硅氧烷、马来酸酐-α-烯烃共聚物与2,2,6,6-四甲基-4-氨基哌啶或1,2,2,6,6-五甲基-4-氨基哌啶的反应产物、2,4-二[N-(1-环己氧基-2,2,6,6-四甲基哌啶-4-基)-N-丁基氨基]-6-(2-羟乙基)氨基-1,3,5-三嗪、1-(2-羟基-2-甲基丙氧基)-4-十八烷酰氧基-2,2,6,6-四甲基哌啶、5-(2-乙基己酰基)氧甲基-3,3,5-三甲基-2-吗啉酮、Sanduvor(Clariant;CAS登记号106917-31-1]、5-(2-乙基己酰基)氧甲基-3,3,5-三甲基-2-吗啉酮、2,4-二[(1-环己氧基-2,2,6,6-哌啶-4-基)丁基氨基]-6-氯-s-三嗪和N,N’-双(3-氨基丙基)乙二胺)的反应产物、1,3,5-三(N-环己基-N-(2,2,6,6-四甲基哌嗪-3-酮-4-基)氨基)-s-三嗪、1,3,5-三(N-环己基-N-(1,2,2,6,6-五甲基哌嗪-3-酮-4-基)氨基)-s-三嗪。
2.7.草酰胺,例如4,4’-二辛氧基N,N’-草酰二苯胺、2,2’-二乙氧基N,N’-草酰二苯胺、2,2’-二辛氧基-5,5’-二叔丁N,N’-草酰二苯胺、2,2’-双十二烷氧基-5,5’-二叔丁N,N’-草酰二苯胺、2-乙氧基-2’-乙基N,N’-草酰二苯胺、N,N’-双(3-二甲基氨基丙基)N,N’-草酰二苯胺、2-乙氧基-5-叔丁基-2’-乙基N,N’-草酰二苯胺及其与2-乙氧基-2’-乙基-5,4’-二叔丁基N,N’-草酰二苯胺的混合物、邻-和对-甲氧基-二取代N,N’-草酰二苯胺混合物以及邻-和对-乙氧基-二取代N,N’-草酰二苯胺混合物。
2.8.2-(2-羟基苯基)-1,3,5-三嗪,例如2,4,6-三(2-羟基-4-辛氧基苯基)-1,3,5-三嗪、2-(2-羟基-4-辛氧基苯基)-4,6-二(2,4-二甲基苯基)-1,3,5-三嗪、2-(2,4-二羟苯基)-4,6-二(2,4-二甲基苯基)-1,3,5-三嗪、2,4-二(2-羟基-4-丙氧基苯基)-6-(2,4-二甲基苯基)-1,3,5-三嗪、2-(2-羟基-4-辛氧基苯基)-4,6-二(4-甲基苯基)-1,3,5-三嗪、2-(2-羟基-4-十二烷氧基苯基)-4,6-二(2,4-二甲基苯基)-1,3,5-三嗪、2-(2-羟基-4-十三烷氧基苯基)-4,6-二(2,4-二甲基苯基)-1,3,5-三嗪、2-[2-羟基-4-(2-羟基-3-丁氧基丙氧基)苯基]-4,6-二(2,4-二甲基)-1,3,5-三嗪、2-[2-羟基-4-(2-羟基-3-辛氧基丙氧基)苯基]-4,6-二(2,4-二甲基)-1,3,5-三嗪、2-[4-(十二烷氧基/十三烷氧基-2-羟基丙氧基)-2-羟基苯基]-4,6-二(2,4-二甲基苯基)-1,3,5-三嗪、2-[2-羟基-4-(2-羟基-3-十二烷氧基丙氧基)苯基]-4,6-二(2,4-二甲基苯基)-1,3,5-三嗪、2-(2-羟基-4-己氧基)苯基-4,6-二苯基-1,3,5-三嗪、2-(2-羟基-4-甲氧基苯基)-4,6-二苯基-1,3,5-三嗪、2,4,6-三[2-羟基-4-(3-丁氧基-2-羟基丙氧基)苯基]-1,3,5-三嗪、2-(2-羟基苯基)-4-(4-甲氧基苯基)-6-苯基-1,3,5-三嗪、2-{2-羟基-4-[3-(2-乙基己基-1-氧)-2-羟基丙氧基]苯基}-4,6-二(2,4-二甲基苯基)-1,3,5-三嗪、2,4-二(4-[2-乙基己氧基]-2-羟基苯基)-6-(4-甲氧基苯基)-1,3,5-三嗪。
3.金属减活剂,例如N,N’-二苯基草酰胺、N-水杨醛-N’-水杨酰肼、N,N’-二(水杨酰基)肼、N,N’-二(3,5-二叔丁基-4-羟基苯基丙酰基)肼、3-水杨酰氨基-1,2,4-三唑、双(亚苄基)草酰二酰肼、N,N’-草酰二苯胺、间苯二甲酰二酰肼、癸二酰二苯基酰肼、N,N’-二乙酰基己二酰二酰肼、N,N’-二(水杨酰基)乙二酰二酰肼、N,N’-二(水杨酰基)硫代丙酰二酰肼。
4.亚磷酸酯和亚膦酸酯,例如亚磷酸三苯酯、亚磷酸二苯基烷基酯、亚磷酸苯基二烷基酯、亚磷酸三(壬基苯基)酯、亚磷酸三(十二烷基)酯、亚磷酸三(十八烷基)酯、双十八烷基季戊四醇二亚磷酸酯、亚磷酸三(2,4-二叔丁基苯基)酯,二异癸基季戊四醇二亚磷酸酯、双(2,4-二叔丁基苯基)季戊四醇二亚磷酸酯、双(2,4-二枯基苯基)季戊四醇二亚磷酸酯、双(2,6-二叔丁基-4-甲基苯基)季戊四醇二亚磷酸酯、二异癸氧基季戊四醇二亚磷酸酯、双(2,4-二叔丁基-6-甲基苯基)季戊四醇二亚磷酸酯、双(2,4,6-三(叔丁基苯基)季戊四醇二亚磷酸酯、三(十八烷基)山梨醇三亚磷酸酯、四(2,4-二叔丁基苯基)-4,4’-联苯撑二亚膦酸酯、6-异辛氧基-2,4,8,10-四叔丁基-12H-二苯并[d,g]-1,3,2-二氧杂磷杂八环(6-isooctyloxy-2,4,8,10-tetra-tert-butyl-12H-dibenz[d,g]-1,3,2-dioxaphosphocin)、亚磷酸-双(2,4-二叔丁基-6-甲基苯基)甲酯、亚磷酸-双(2,4-二叔丁基-6-甲基苯基)乙酯、6-氟-2,4,8,10-四叔丁基-12-甲基-二苯并[d,g]-1,3,2-二氧杂磷杂八环、2,2’,2”-次氮基[三乙基三(3,3’,5,5’-四叔丁基-1,1’-联苯-2,2’-二基)亚磷酸酯]、2-乙基己基(3,3’,5,5’-四叔丁基-1,1’-联苯-2,2’-二基)亚磷酸酯、5-丁基-5-乙基-2-(2,4,6-三叔丁基苯氧基)-1,3,2-二氧杂磷杂八环。
特别优选下列亚磷酸酯:
5.羟胺,例如N,N-二苄基羟胺、N,N-二乙基羟胺、N,N-二辛基羟胺、N,N-双十二烷基羟胺、N,N-双十四烷基羟胺、N,N-双十六烷基羟胺、N,N-双十八烷基羟胺、N-十六烷基-N-十八烷基羟胺、N-十七烷基-N-十八烷基羟胺、由氢化牛脂胺得到的N,N-二烷基羟胺。
6.硝酮,例如N-苄基-α-苯基硝酮、N-乙基-α-甲基硝酮、N-辛基-α-庚基硝酮、N-十二烷基-α-十一烷基硝酮、N-十四烷基-α-十三烷基硝酮、N-十六烷基-α-十五烷基硝酮、N-十八烷基-α-十七烷基硝酮、N-十六烷基-α-十七烷基硝酮、N-十八烷基-α-十五烷基硝酮、N-十七烷基-α-十七烷基硝酮、N-十八烷基-α-十六烷基硝酮、由N,N-二烷基羟胺得到的硝酮,所述N,N-二烷基羟胺由氢化牛脂胺得到。
7.硫代增效剂,例如硫代二丙酸双十二烷基酯、dimistrylthiodipropionate、硫代二丙酸双十八烷基酯或双十八烷基二硫化物。
8.过氧化物清除剂,例如β-硫代二丙酸的酯,如十二烷基酯、十八烷基酯、十四烷基酯或十三烷基酯、巯基苯并咪唑或2-巯基苯并咪唑的锌盐、二丁基二硫代氨基甲酸锌、双十八烷基二硫化物、季戊四醇-四(β-十二烷基巯基)丙酸酯。
9.聚酰胺稳定剂,例如铜盐与碘化物和/或磷化合物及二价锰盐的组合。
10.碱性共稳定剂,例如三聚氰胺、聚乙烯吡咯烷酮、双氰胺、三烯丙基氰尿酸酯、脲衍生物、肼衍生物、胺、聚酰胺、聚氨酯、高级脂肪酸的碱金属和碱土金属盐,例如硬脂酸钙、硬脂酸锌、山萮酸镁、硬脂酸镁、蓖麻酸钠和棕榈酸钾、邻苯二酚锑或邻苯二酚锌。
11.成核剂,例如无机物,如滑石、金属氧化物如二氧化钛或氧化镁、优选碱土金属的磷酸盐、碳酸盐或硫酸盐;有机物,如一元或多元羧酸及其盐,例如4-叔丁基苯甲酸、己二酸、二苯基乙酸、琥珀酸钠或苯甲酸钠;聚合物,如离子型共聚物(离聚物)。特别优选1,3:2,4-二(3’,4’-二甲基亚苄基)山梨醇、1,3:2,4-二(对甲基二亚苄基)山梨醇、和1,3:2,4-二亚苄基山梨醇。
12.填料和增强剂,例如碳酸钙、硅酸盐、玻璃纤维、玻璃珠、石棉、滑石、高岭土、云母、硫酸钡、金属氧化物和氢氧化物、炭黑、石墨、木粉和其它天然产品的粉末或纤维、合成纤维。
13.其它添加剂,例如增塑剂、润滑剂、乳化剂、颜料、流变添加剂、催化剂、流量控制剂、荧光增白剂、阻燃剂、抗静电剂和发泡剂。
14.苯并呋喃酮和吲哚酮,例如美国专利4,325,863、美国专利4,338,244、美国专利5,175,312、美国专利5,216,052、美国专利5,252,643;德国专利DE-A-4316611、德国专利DE-A-4316622、德国专利DE-A-4316876、欧洲专利EP-A-0589839、欧洲专利EP-A-0591102、欧洲专利EP-A-1291384中所公开的那些或3-[4-(2-乙酰氧基乙氧基)苯基]-5,7-二叔丁基苯并呋喃-2-酮、5,7-二叔丁基-3-[4-(2-硬脂酰氧基乙氧基)苯基]苯并呋喃-2-酮、3,3’-二[5,7-二叔丁基-3-(4-[2-羟基乙氧基]苯基)苯并呋喃-2-酮],5,7-二叔丁基-3-(4-乙氧基苯基)苯并呋喃-2-酮、3-(4-乙酰氧基-3,5-二甲基苯基)-5,7-二叔丁基苯并呋喃-2-酮、3-(3,5-二甲基-4-新戊酰氧基苯基)-5,7-二叔丁基苯并呋喃-2-酮、3-(3,4-二甲基苯基)-5,7-二叔丁基苯并呋喃-2-酮、3-(2,3-二甲基苯基)-5,7-二叔丁基苯并呋喃-2-酮、3-(2-乙酰基-5-异辛基苯基)-5-异辛基苯并呋喃-2-酮。
如果含有常规添加剂和其它抗微生物剂,基于所述聚合物材料的重量,其含量通常在0.001到10重量%,特别是0.01到5重量%。
根据本发明的优选的抗微生物聚合物或涂料还包含例如一种或多种选自其它抗微生物剂、抗氧化剂、光稳定剂如紫外线吸收剂和/或立体受阻胺、亚磷酸盐、亚膦酸盐、成核剂、填料、增塑剂、颜料、阻燃剂、抗静电剂的成分,其例子如上所列。
所述聚合物或塑料可以以任何形式存在,例如纤维、薄膜或模制部件。它们可以是例如纺织或无纺的高分子织物。
通常,本发明的具有抗微生物活性的塑料可以选自:
1.单烯烃或二烯烃的聚合物,例如聚丙烯、聚异丁烯、聚丁-1-烯、聚-4-甲基戊-1-烯、聚异戊二烯或聚丁二烯,以及环烯烃聚合物,例如环戊烯或降冰片烯,聚乙烯(可选交联),例如高密度聚乙烯(HDPE)、低密度聚乙烯(LDPE)、线性低密度聚乙烯(LLDPE)、支化低密度聚乙烯(BLDPE)及中密度聚乙烯(MDPE)。
聚烯烃,即在上一段中举例的单烯烃的聚合物,优选聚乙烯和聚丙烯,其可以通过不同方法制备,特别是通过下列方法:
a)自由基聚合(通常在高压高温下)。
b)利用催化剂的催化聚合,所述催化剂通常包含一种或多种元素周期表中第IVb、Vb、VIb或VIII族的金属。这些金属通常具有一种或多种配体,代表性地为可以p-或s-配位的氧化物、卤化物、醇化物、酯、醚、胺、烷基、烯基和/或芳基。这些金属配合物可以以游离形式存在或者固定在基质上,代表性地固定在活化氯化镁、氯化钛(III)、氧化铝或氧化硅上。这些催化剂可溶或不溶于聚合介质中。这些催化剂可以在聚合中单独使用,也可使用其它激活剂,其代表为烷基金属、金属氢化物、烷基金属卤化物、烷基金属氧化物或金属烷基噁烷,所述金属为元素周期表中第Ia,IIa和/或IIIa族的元素。所述激活剂可以方便地用其它酯、醚、胺或硅醚基团改性。这些催化剂体系通常被称为Phillips、Standard Oil Indiana、Ziegler(-Natta)、TNZ(DuPont)、茂金属或单活性中心催化剂(SSC)。
2.1)中所提到的聚合物的混合物,例如聚丙烯和聚异丁烯的混合物、聚丙烯和聚乙烯的混合物(例如PP/HDPE,PP/LDPE)及不同种类聚乙烯的混合物(例如LDPE/HDPE)。
3.单烯烃和二烯烃彼此之间或与其它乙烯基单体的共聚物,例如乙烯/丙烯共聚物、线性低密度聚乙烯(LLDPE)及其与低密度聚乙烯(LDPE)的混合物、丙烯/丁-1-烯共聚物、丙烯/异丁烯共聚物、乙烯/丁-1-烯共聚物、乙烯/己烯共聚物、乙烯/甲基戊烯共聚物、乙烯/庚烯共聚物、乙烯/辛烯共聚物、丙烯/丁二烯共聚物、异丁烯/异戊二烯共聚物、乙烯/丙烯酸烷基酯共聚物、乙烯/甲基丙烯酸烷基酯共聚物、乙烯/醋酸乙烯酯共聚物及其与一氧化碳的共聚物或乙烯/丙烯酸共聚物及其盐(离聚物),以及乙烯与丙烯和二烯烃如己二烯、二环戊二烯或亚乙基-降冰片烯的三元共聚物;以及这些共聚物彼此之间及其与1)所提及的聚合物的混合物,例如聚丙烯/乙烯-丙烯共聚物、LDPE/乙烯-醋酸乙烯酯共聚物(EVA)、LDPE/乙烯-丙烯酸共聚物(EAA)、LLDPE/EVA、LLDPE/EAA和交替或无规聚烯烃/一氧化碳共聚物及其与其它聚合物如聚酰胺的混合物。
4.烃树脂(例如C5-C9),包括其氢化改性物(如增粘剂)及聚烯烃和淀粉的混合物。
5.聚苯乙烯、聚对甲基苯乙烯、聚(α-甲基苯乙烯)。
6.苯乙烯或α-甲基苯乙烯与二烯烃或丙烯酸衍生物的共聚物,例如苯乙烯/丁二烯、苯乙烯/不饱和酯、苯乙烯/丙烯腈、苯乙烯/甲基丙烯酸烷基酯、苯乙烯/丁二烯/丙烯酸烷基酯、苯乙烯/丁二烯/甲基丙烯酸烷基酯、苯乙烯/马来酸酐、苯乙烯/丙烯腈/丙烯酸甲酯;高冲击强度苯乙烯共聚物与另一种聚合物如聚丙烯酸酯、二烯烃聚合物或乙烯/丙烯/二烯烃三元共聚物的混合物;以及苯乙烯的嵌段共聚物如苯乙烯/丁二烯/苯乙烯、苯乙烯/异戊二烯/苯乙烯、苯乙烯/乙烯/丁烯/苯乙烯或苯乙烯/乙烯/丙烯/苯乙烯。
7.苯乙烯或α-甲基苯乙烯的接枝共聚物,例如聚丁二烯接枝苯乙烯、聚丁二烯-苯乙烯或聚丁二烯-丙烯腈共聚物接枝苯乙烯;聚丁二烯接枝苯乙烯和丙烯腈(或甲基丙烯腈);聚丁二烯接枝苯乙烯、丙烯腈和甲基丙烯酸甲酯;聚丁二烯接枝苯乙烯和马来酸酐;聚丁二烯接枝苯乙烯、丙烯腈和马来酸酐或马来酰亚胺;聚丁二烯接枝苯乙烯和马来酰亚胺;聚丁二烯接枝苯乙烯和丙烯酸或甲基丙烯酸烷基酯;乙烯/丙烯/二烯烃三元共聚物接枝苯乙烯和丙烯腈;聚丙烯酸烷基酯或聚甲基丙烯酸烷基酯接枝苯乙烯和丙烯腈、丙烯酸酯/丁二烯共聚物接枝苯乙烯和丙烯腈,及其与6)所列共聚物的混合物,例如已知的被称为ABS,SAN,MBS,ASA或AES聚合物的共聚物混合物。
8.含卤素聚合物如聚氯丁烯、氯化橡胶、氯化或氯磺化聚乙烯、乙烯和氯化乙烯的共聚物、表氯醇均聚物或共聚物,特别是含卤素乙烯基化合物的聚合物,例如聚氯乙烯、聚偏二氯乙烯、聚氟乙烯、聚偏二氟乙烯,及其共聚物如氯乙烯/偏二氯乙烯、氯乙烯/醋酸乙烯酯或偏二氯乙烯/醋酸乙烯酯共聚物。
9.由α,β-不饱和酸及其衍生物得到的聚合物,例如聚丙烯酸酯和聚甲基丙烯酸酯;用丙烯酸丁酯进行冲击改性的聚甲基丙烯酸甲酯、聚丙烯酰胺和聚丙烯腈。
10.9)所述单体彼此之间或其与其它不饱和单体的共聚物,例如丙烯腈/丁二烯共聚物、丙烯腈/丙烯酸烷基酯共聚物、丙烯腈/丙烯酸烷氧基烷基酯或丙烯腈/卤代乙烯共聚物或丙烯腈/甲基丙烯酸烷基酯/丁二烯三元共聚物。
11.由不饱和醇和胺或其酰基衍生物或缩醛得到的聚合物,例如聚乙烯醇、聚乙酸乙烯酯、聚硬脂酸乙烯酯、聚苯甲酸乙烯酯、聚马来酸乙烯酯、聚乙烯醇缩丁醛、聚苯二甲酸烯丙酯或聚烯丙基三聚氰胺;及其与上述1)所提及的烯烃的共聚物。
12.环醚的均聚物和共聚物,例如聚烷撑二醇、聚环氧乙烷、聚环氧丙烷或其与二缩水甘油醚的共聚物。
13.聚缩醛如聚甲醛及那些含有环氧乙烷作为共聚单体的聚甲醛;用热塑性聚氨酯、丙烯酸酯或MBS改性的聚缩醛。
14.聚苯醚和聚苯硫醚,以及聚苯醚与苯乙烯聚合物或聚酰胺的混合物。
15.一方面衍生自端羟基聚醚、聚酯或聚丁二烯而另一方面衍生自脂肪族或芳香族多异氰酸酯的聚氨酯及其前体。
16.衍生自二元胺和二元羧酸和/或衍生自氨基羧酸或相应内酰胺的聚酰胺和共聚酰胺,例如聚酰胺4、聚酰胺6、聚酰胺6/6、6/10、6/9、6/12、4/6、12/12、聚酰胺11、聚酰胺12、由间二甲苯二胺和己二酸得到的芳香族聚酰胺;由六亚甲基二胺和间苯二甲酸或/和对苯二甲酸和任选的作为改性剂的弹性体制备的聚酰胺,例如聚-2,4,4,-三甲基六亚甲基对苯二甲酰胺或聚-间亚苯基间苯二酰胺;以及上述聚酰胺与聚烯烃、烯烃共聚物、离聚物或化学键合或接枝弹性体的嵌段共聚物;或者与聚醚例如聚乙二醇、聚丙二醇或聚四亚甲基二醇的共聚物;以及用EPDM或ABS改性的聚酰胺或共聚酰胺;和在加工过程中缩合的聚酰胺(RIM聚酰胺体系)。
17.聚脲、聚酰亚胺、聚酰胺-酰亚胺和聚苯并咪唑。
18.衍生自二羧酸和二醇和/或羟基羧酸或相应内酯的聚酯,例如聚对苯二甲酸乙二醇酯、聚对苯二甲酸三亚甲基二醇酯、聚对苯二甲酸丁二醇酯、聚对苯二甲酸-1,4-二羟甲基环己烷酯和聚羟基苯甲酸酯,以及衍生自端羟基聚醚的嵌段共聚醚酯;和用聚碳酸酯或MBS改性的聚酯。美国专利第5,807,932号(第2列,第53行)定义的聚酯和聚酯共聚物,通过引用并入本文。
19.聚碳酸酯和聚酯碳酸酯。
20.聚砜、聚醚砜和聚醚酮。
21.一方面衍生自醛而另一方面衍生自苯酚、脲和三聚氰胺的交联聚合物,如苯酚/甲醛树脂、脲/甲醛树脂和三聚氰胺/甲醛树脂。
22.干燥或非干燥醇酸树脂。
23.衍生自饱和及不饱和二羧酸并以多元醇和乙烯基化合物作为交联剂的共聚酯的不饱和聚酯树脂,及其具有低可燃度的含卤素改性产物。
24.可交联丙烯酸树脂,衍生自取代丙烯酸酯例如环氧丙烯酸酯、聚氨酯丙烯酸酯(urethane acrylate)或聚酯丙烯酸酯。
25.与三聚氰胺树脂、脲醛树脂、多异氰酸酯或环氧树脂交联的醇酸树脂、聚酯树脂和丙烯酸酯树脂。
26.交联环氧树脂,衍生自聚环氧化物例如双缩水甘油醚或脂环族二环氧化物。
27.天然聚合物如纤维素、橡胶、明胶及其化学改性同系衍生物,例如醋酸纤维素、丙酸纤维素和丁酸纤维素,或纤维素醚如甲基纤维素;以及松香及其衍生物。
28.上述聚合物的混合物(聚合物共混物),例如PP/EPDM、聚酰胺/-EPDM或ABS、PVC/EVA、PVC/ABS、PVC/MBS、PC/ABS、PBTP/ABS、PC/ASA、PC/PBT、PVC/CPE、PVC/丙烯酸酯、POM/热塑性PUR、PC/热塑性PUR、POM/丙烯酸酯、POM/MBS、PPO/HIPS、PPO/PA 6.6及共聚物、PA/HDPE、PA/PP、PA/PPO。
29.自然产生及合成有机材料,其为纯单体化合物或所述化合物的混合物,例如矿物油、动物和植物脂肪、油和蜡、或者基于合成酯(例如苯二甲酸酯、己二酸酯、磷酸酯或偏苯三酸酯)的油、脂肪和蜡、以及合成酯与矿物油以任何重量比的混合物,其代表为那些用作纺丝组合物的物质,以及这些材料的水乳化液。
30.天然或合成橡胶的水乳化液,例如天然胶乳或羧酸化苯乙烯/丁二烯共聚物的胶乳。
31.聚硅氧烷,比如在例如美国专利第4,259,467号中所述的软亲水性聚硅氧烷,以及在例如美国专利第4,355,147号中所述的硬聚硅氧烷。
32.硅氧烷弹性体,例如液体硅橡胶(LSR)。所述液体硅橡胶可由DowChemical提供,并在例如美国专利第6,569,53、6,420,038、6,297,291、6,218,466、6,130,272、5,994,461、5,989,719、5,973,030、5,908,888、5,880,199、5,877,256、5,859,094、5,789,084和5,661,210号中有所描述。这些美国专利的公开内容通过引用并入本文。
33.聚酮亚胺与不饱和丙烯酸聚乙酰乙酸酯树脂或不饱和丙烯酸树脂的组合。所述不饱和丙烯酸树脂包括聚氨酯丙烯酸酯、聚醚丙烯酸酯、具有不饱和侧基的乙烯基或丙烯醛基共聚物以及丙烯酸化三聚氰胺。所述聚酮亚胺由聚胺和酮在酸催化剂的作用下制备。
34.包含乙烯系不饱和单体或低聚物以及多不饱和脂肪族低聚物的辐射固化组合物。
35.环氧三聚氰胺树脂,比如用环氧官能共醚化高固含量三聚氰胺树脂如LSE-4103(Monsanto)交联的光稳定环氧树脂。
也包括热塑性烯烃(TPO),热塑性弹性体、聚醚酰亚胺、聚甲基戊烯、聚苯醚、聚苯硫醚、聚砜或聚四氟乙烯(PTFE)。具有特别的优良技术效果的一些聚合物包括:
聚砜(PSF)
聚醚砜(PES)
聚苯砜(PPS)
聚偏二氟乙烯(PVDF)
聚丙烯(PP)
聚乙烯(PE)
纤维素、醋酸纤维素(CA)、硝酸纤维素
聚酰胺(PA)
聚丙烯腈(PAN)
聚四氟乙烯(PTFE)
聚碳酸酯(PC)
聚甲基丙烯酸甲酯(PMMA)。
特别地,所述聚合物是那些典型地用于医药用途的物质,例如聚氨酯、聚碳酸酯、液体硅橡胶、聚乙烯、聚丙烯、聚乙烯/聚丙烯共聚物或聚合物复合材料。
所述聚合物复合材料为例如天然产品复合材料,例如与热塑性聚合物如聚烯烃混合的天然产品。已公布的美国申请第20040235983号中公开了这些复合材料,其公开内容通过引用并入本文。所述天然产品为例如木粉、亚麻、麻、黄麻、洋麻或谷皮。所述热塑性聚合物为例如聚乙烯或聚丙烯。
本发明的抗微生物银添加剂可以单独或彼此混合加入聚合物基质中。如果需要,在掺入所述聚合物中之前,这些单独成分可以通过例如干法混合而彼此混合。
可以通过公知方法掺入本发明的银添加剂,例如粉末形式的干法混合,或者在例如惰性溶剂、水或油中的溶液、分散体或悬浮液形式的湿法混合。本发明的添加剂可以例如在成型之前或之后掺入,或者通过将溶解的或分散的添加剂或添加剂混合物加入所述聚合物材料中,在此之后蒸发或不蒸发溶剂或悬浮/分散剂。它们可以以干混合物或粉末或者以溶液或分散体或悬浮液的形式直接加入处理装置(如挤出机、密炼机等等)中。
所述掺入可以在任何配有搅拌器的可加热容器中进行,例如在封闭装置如捏合机、混合器或搅拌釜中。所述掺入优选在挤出机或捏合机中进行。该处理过程可以在惰性气氛或氧气存在下进行。
向聚合物基质中加入所述银添加剂可以在任何常规混合机中进行,在其中所述聚合物被熔化并与所述添加剂混合。适合的机器为本领域技术人员所公知。它们主要是混合器、捏合机和挤出机。
所述处理包括挤出、共捏合(co-kneading)、拉挤、模压成型、片材挤出、热成型、注射成型或旋转成型。该处理优选通过在处理过程中加入所述添加剂在挤出机中进行。
特别优选的处理机器是单螺杆挤出机、对向旋转或同向旋转双螺杆挤出机、旋转成型设备、行星齿轮挤出机、环式挤出机或共捏合机。也可以利用具有至少一个可以被施加真空的脱气室的处理机器。
适合的挤出机和捏合机在例如Handbuch der Kunststoffextrusion,Vol.1 Grundlagen,Editors F.Hensen,W.Knappe,H.Potente,1989,pp.3-7,ISBN:3-446-14339-4(Vol.2 Extrusionsanlagen 1986,ISBN 3-446-14329-7)中有所描述。
例如,所述螺杆长度是螺杆直径的1-60倍,优选螺杆直径的35-48倍。所述螺杆转速优选10-600转每分(rpm),特别优选25-300rpm。
最大处理量由螺杆直径、转速和驱动力决定。本发明的过程也可以通过改变所提及的参数或利用称重机配送剂量,以低于最大处理量的程度进行。
所述银添加剂可以预混合或单独添加。
也可以将本发明的银添加剂加入母料(“浓缩物”)形式的聚合物中,该母料包含所述组分的浓度为例如以掺入聚合物重量计大约1%到大约40%,优选大约2%到大约20%。该聚合物并不必须与所述添加剂最终加入的聚合物一致。在这个操作中,所述聚合物可以以粉末、颗粒、溶液、悬浮液或胶乳形式使用。
掺入可以在成型操作之前或期间进行,或通过将分散的化合物加入所述聚合物中,在之后蒸发或不蒸发溶剂。另外一种将本发明的添加剂掺入聚合物基质的可能是将其在相应单体聚合之前、聚合期间或直接在聚合之后加入或者在交联之前加入。在这种情况下,可以直接或以胶囊形式(例如在蜡、油或聚合物中)加入本发明的添加剂。
这里所述的含有本发明的添加剂的聚合物可以用于生产模制品、旋转成型制品、注射成型制品、吹塑制品、型材、薄膜、纺织或无纺布,等等。
当所述塑料制品用于医疗领域时,其为例如导管(catheter)、软管(hose)、管(tube)、阀、泌尿学用品、骨接合剂、织物、牙刷、有机硅塑料、膜、纺织品、尿布等等。
本发明的涂料包含成膜粘合剂。
所述粘合剂原则上可以是任何工业上惯用的粘合剂,例如Ullmann′sEncyclopedia of Industrial Chemistry,5th Edition,Vol.A18,pp.368-426,VCH,Weinheim 1991中所述的那些粘合剂。通常,其为基于热塑性或热固性树脂,优选热固性树脂的成膜粘合剂。例如醇酸、丙烯酸、丙烯酸醇酸、聚酯、酚醛、三聚氰胺、环氧和聚氨酯树脂及其混合物。
所述粘合剂可以为可冷固化或可热固化粘合剂;加入固化促进剂可能对其有利。该粘合剂的合适的固化促进剂在例如Ullmann′s Encyclopediaof Industrial Chemistry,Vol.A18,p.469,VCH Verlagsgesellschaft,Weinheim 1991中有所描述。
所述涂料可用作例如塑料或金属的表涂层或作为木材涂层。
含有特定粘合剂的所述涂料组合物的例子包括:
1.基于可冷或热交联醇酸、丙烯酸酯、聚酯、环氧或三聚氰胺树脂或这些树脂的混合物的涂料,如果需要加入固化促进剂;
2.基于含羟基丙烯酸酯、聚酯或聚醚树脂及脂肪族或芳香族异氰酸酯、异氰尿酸酯或多异氰酸酯的双组分聚氨酯涂料;
3.基于在烘焙期间去封闭的封闭型异氰酸酯、异氰尿酸酯或多异氰酸酯的单组分聚氨酯涂料,如果需要加入三聚氰胺树脂;
4.基于三烷氧羰基三嗪交联剂和如丙烯酸酯、聚酯或聚醚树脂的含羟基树脂的单组分聚氨酯涂料;
5.基于在氨基甲酸酯结构中具有游离氨基的脂肪族或芳香族氨基甲酸酯丙烯酸酯或聚氨酯丙烯酸酯及三聚氰胺树脂或聚醚树脂的单组分聚氨酯涂料,如果需要加入固化促进剂;
6.基于(聚)酮亚胺和脂肪族或芳香族异氰酸酯、异氰尿酸酯或多异氰酸酯的双组分涂料;
7.基于(聚)酮亚胺和不饱和丙烯酸酯树脂或聚乙酰乙酸酯树脂或甲基丙烯酰氨基乙醇酸酯甲酯的双组分涂料;
8.基于含羧基或含氨基的聚丙烯酸酯或聚环氧化物的双组分涂料;
9.基于含酸酐基团的丙烯酸酯树脂和多羟基或多氨基组分的双组分涂料;
10.基于含丙烯酸酯酸酐和聚环氧化物的双组分涂料;
11.基于(聚)噁唑啉和含酸酐基团的丙烯酸酯树脂、或不饱和丙烯酸酯树脂、或脂肪族或芳香族异氰酸酯、异氰尿酸酯或多异氰酸酯的双组分涂料;
12.基于不饱和聚丙烯酸酯和聚丙二酸酯的双组分涂料;
13.基于与醚化三聚氰胺树脂结合的热塑性丙烯酸酯树脂或外交联丙烯酸酯树脂的热塑性聚丙烯酸酯涂料;
14.基于硅氧烷改性或氟改性丙烯酸酯树脂的涂料体系。
所述涂料组合物也可以包括其他成分,例如溶剂、颜料、染料、增塑剂、稳定剂、触变剂、干燥催化剂和/或均化剂。可能的成分的例子在Ullmann′s Encyclopedia of Industrial Chemistry,5th Edition,Vol.A18,pp.429-471,VCH,Weinheim 1991中有所描述。
例如,可能的干燥催化剂或固化促进剂为例如有机金属化合物、胺、含氨基树脂和/或膦。所述有机金属化合物的例子为金属羧酸盐,特别是Pb、Mn、Co、Zn、Zr或Cu的羧酸盐,或金属螯合物,特别是Al、Ti或Zr的螯合物,或有机金属化合物如有机锡化合物。
所述金属羧酸盐的例子为Pb、Mn或Zn的硬脂酸盐、Co、Zn或Cu的辛酸盐、Mn和Co的环烷酸盐或相应的亚油酸盐、树脂酸盐或脂肪酸盐。
所述金属螯合物的例子为乙酰丙酮、乙酰乙酸乙酯、水杨醛、水杨醛肟、邻羟基苯乙酮或三氟乙酰乙酸乙酯的铝、钛或锆螯合物,以及这些金属的醇盐。
所述有机锡化合物的例子为二丁基氧化锡、二月桂酸二丁基锡或二辛酸二丁基锡。
特别地,所述胺的例子为叔胺,例如三丁基胺、三乙醇胺、N-甲基二乙醇胺、N-二甲基乙醇胺、N-乙基吗啉、N-甲基吗啉或二氮杂二环辛烷(三亚乙基二胺)及其盐。其它例子如季铵盐,例如三甲基苄基氯化铵。
含氨基树脂同时为粘合剂和固化促进剂。其例子为含氨基丙烯酸酯共聚物。
所用固化促进剂也可以为膦,例如三苯基膦。
所述涂料组合物也可以是辐射固化涂料组合物。在此情况下,所述粘合剂主要包括含乙烯性不饱和键的单体或低聚化合物,其在使用后通过光化辐射进行固化,即转化为交联的高分子量形式。当该体系为紫外光固化时,其一般还包含光引发剂。在上述出版物Ullmann′s Encyclopedia ofIndustrial Chemistry,5th Edition,Vol.A18,pages 451-453中描述了相应的体系。
本发明的涂料组合物可以用于任何需要的基质,例如金属、木材、塑料、陶瓷材料或塑木复合材料。
也公开了所述涂料组合物用于保护木材表面的用途,例如通过将所述银添加剂掺入木材上的清漆、涂料、着色剂或浸渍剂。本发明因此也涉及用于赋予木材表面以抗微生物活性的方法,该方法包括将所述涂料组合物施加到特别是木材上的清漆、涂料或浸渍剂中。所述银成分可以作为着色剂或浸渍剂的部分或作为表涂层的部分施加。
如果所述木材涂层为着色剂或浸渍剂,优选使用选自脂肪烃、脂环烃、芳烃、醇、醚、酯、酮、乙二醇、乙二醇醚、乙二醇酯、聚乙二醇或其混合物的溶剂。在这种情况下所述粘合剂优选选自醇酸树脂、改性醇酸树脂、自交联或非自交联丙烯酸树脂、聚酯树脂、干燥油、酚树脂、硝酸纤维素或其混合物。
可以使用其它添加剂如杀真菌剂或杀虫剂。有用的杀真菌剂的例子为三丁基氧化锡,苯基汞盐、环烷酸铜、1-氯萘或五氯苯酚。有用的杀虫剂的例子为DDT、狄氏剂、林丹、azaconazol、cypermethin、benzalkoniumhydrochloride、丙环唑或对硫磷。
任何适于涂覆木材的涂料组合物可以用作表涂层。其通常包含溶解或分散于有机溶剂或水或水与溶剂的混合物中的粘合剂。该粘合剂可以代表性地为在空气中干燥或在室温下硬化的表面涂覆树脂。这种粘合剂的例子为硝酸纤维素、聚乙酸乙烯酯、聚氯乙烯、不饱和聚酯树脂、聚丙烯酸酯、聚氨酯、环氧树脂、酚醛树脂、和特别是醇酸树脂。该粘合剂也可以是不同表面涂覆树脂的混合物。如果该粘合剂为可固化粘合剂,其通常与硬化剂和/或促进剂一同使用。
所述表涂层也可以为光可聚合化合物的辐射固化的无溶剂配方。其例子为丙烯酸酯或甲基丙烯酸酯的混合物、不饱和聚酯/苯乙烯混合物或其它乙烯基不饱和单体或低聚体的混合物。
所述表涂层可以包含可溶性染料和/或颜料和/或填料。所述颜料可以为有机、无机或金属颜料。所述颜料可以是不透明的,也可以是透明的,例如透明氧化铁。所述填料可以代表性地为高岭土、碳酸钙或硅酸铝。所述表涂层优选为透明清漆,即其不包含不溶成分。
本发明在下列应用中特别有用:在家用中,如家具、木地板、刨花板或木质结构;在室外应用如栅栏、施工件、木质前缘、窗框等等。
可以通过常规方法将所述涂料组合物施加到所述基质上,例如通过刷、喷射、浇注、浸渍或电泳;也见Ullmann′s Encyclopedia of IndustrialChemistry,5th Edition,Vol.A18,pp.491-500。
由所述粘合剂体系而定,该涂料可以在室温下或通过加热固化。该涂料可以例如在50-150℃下固化,并且在粉末涂料或卷材涂料的情况下甚至需要更高的温度。
所述涂料组合物可以包括可溶解所述粘合剂的有机溶剂或溶剂混合物。所述涂料组合物也可以为水溶液或水分散体。该载体也可以为有机溶剂和水的混合物。所述涂料组合物可以为高固含量涂料或无溶剂(如粉末涂料材料)。所述粉末涂料为例如那些在Ullmann’s Encyclopedia of IndustrialChemistry,5th Ed.,A18,pages 438-444中所述的物质。所述粉末涂料材料也可以具有粉-浆形式(优选在水中的粉末分散体)。
所述颜料可以是无机、有机或金属颜料。所述涂料组合物可以不包含颜料,也可以用作透明涂料。
在固化所述涂料以前的任意时间点,同时或分别向所述涂料组合物中简单加入所述银添加剂。
实施例
下列实施例进一步阐明了本发明。除非另外说明,量以重量%计。关于所述带有载体的银,所述重量%以银为基础。室温通常表示从20-25℃范围内的温度。
实施例1
翻滚混合聚丙烯以包含0.01或0.1重量%的元素银,和0.001或0.01重量%的负载于沸石或玻璃上的银,以聚合物的重量为基础。
这些混合物用Leistritz 27mm双螺杆挤出机单独复合。在水槽中冷却所述熔化物,并通过Conair-Jetro Model 304造粒机将线转化为颗粒。
所述无纺织物显示突出的抗微生物活性。
实施例2
将基于树脂固体重量的1重量%的元素银和0.1重量%的负载于沸石或玻璃上的银掺入以市售聚酯多元醇和市售异氰尿酸酯为基础的双组分聚酯聚氨酯涂料中。用基于总树脂固体量0.015%的二月桂酸二丁基锡催化所述涂料体系。
向大约4”x6”的透明载玻片通过刮涂(drawdown)施加所述涂料配方直至膜厚为大约2密耳(0.002”)。
在120°F(49℃)烘箱中固化这些薄膜。
所述聚酯聚氨酯薄膜显示突出的抗微生物活性。
实施例3
将薄膜级聚乙烯与适当量的所述银添加剂进行干混,并在200℃下熔融复合而得到“母料”颗粒。将该充分配制的“母料”颗粒与聚乙烯树脂进行干混而得到所要的最终稳定剂浓度。代表性的配方包含大约2%的元素银和大约0.02%的带有载体的银、0.05%到0.5%的金属硬脂酸盐例如硬脂酸钙、0%到0.1%的亚磷酸酯、0%到1.25%的酚类抗氧剂、0%到0.1%的N,N-二烷基羟胺和可选地0%到2.0%的受阻胺。然后在DOLCI薄膜生产线上将这种稳定化的充分配制的树脂在200℃下吹制成为150微米厚的薄膜。
所述PE薄膜显示突出的抗微生物活性。
实施例4
将聚氨酯颗粒与1重量%的元素银和0.04重量%的负载于沸石或玻璃上的银混合。将所述颗粒挤出并压模成为125密耳的薄片。
所述聚氨酯片显示突出的抗微生物活性。
实施例5
根据美国专利第5,973,030号所述制备液体硅橡胶薄板。所述配方还进一步包括0.01到1重量%的元素银和0.001到0.01重量%的负载于沸石或玻璃上的银。例如,使用了1.2重量%的元素银和0.05重量%的负载于沸石或玻璃上的银。
所述薄板显示突出的抗微生物活性。
实施例6
将包含1重量%的元素银和0.06重量%的负载于沸石或玻璃上的银的水基透明透明丙烯酸工业涂料配方以2密耳的厚度涂覆在载玻片上。
所述涂覆载玻片显示突出的抗微生物活性。
实施例7
制备包含1重量%的元素银和0.04重量%的负载于沸石或玻璃上的银的溶剂型聚氨酯涂料。将所述涂料以2密耳的厚度施加在载玻片上。
所述涂覆载玻片显示突出的抗微生物活性。
实施例8
通过用高速搅拌机混合所述组分(见下表)来配制透明的可紫外固化水性工业涂料。
重量% | |
Alberdingk Lux 399(丙烯酸酯-聚氨酯共聚物分散体),Alberdingk Boley | 98.3 |
Borchigel L 75N(增稠剂),Borchers | 0.3 |
Byk 347(润湿剂),Byk Chemie | 0.4 |
IRGACURE 500(光引发剂),Ciba | 1.0 |
向所制备的配方中加入元素银(总配方0.5重量%的银)和负载于沸石或玻璃上的银(总配方0.005重量%的银),并在室温下以高剪切速率(2000rpm)搅拌30分钟。为了进行对照,用同样方法制备仅仅含有元素银、仅仅含有带有载体的银、或完全不含银的对照配方。
用50μm狭缝涂布机将所述涂料施加到白色涂覆铝面板上,在60℃下干燥10分钟,并用两个中压汞蒸汽灯(2x80W/cm)在5m/min下固化以用于微生物测试。
实施例9
根据下列步骤制备双组分溶剂型聚氨酯涂料:
向作为研磨基料配方的粘合剂和溶剂中加入元素银(研磨基料配方的5重量%)和负载于沸石或玻璃上的银(研磨基料配方的5重量%),并在高剪切速率下搅拌10分钟直至达到颗粒度小于5μm。
研磨基料配方:
重量% | |
Macrynal SM 510n(在10%芳烃、20%二甲苯、10%乙酸正丁酯中的60%的丙烯酸共聚物) | 79.0 |
乙酸丁二醇酯(溶剂) | 11.0 |
含银沸石或玻璃(1.1%) | 5.0 |
元素银 | 5.0 |
总和 | 100.0 |
通过混合组分A的成分并最后在使用前加入组分B制备所述涂料配方(见下表)。元素银在总配方中的含量为1重量%的银,而负载于沸石或玻璃上的银在总配方中的含量为0.011重量%的银。
涂料配方:
组分A: | 重量% |
研磨基料 | 28.0 |
Macrynal SM 510n(在10%芳烃、20%二甲苯、10%乙酸正丁酯中的60%的丙烯酸共聚物) | 52.3 |
乙酸丁二醇酯(溶剂) | 9.7 |
Solvesso 100(芳烃混合物) | 6.2 |
甲基异丁基酮(溶剂) | 3.6 |
Byk 300(聚醚改性二甲基聚硅氧烷-共聚物在二甲苯/异丁醇(4/1)中的52%溶液) | 0.2 |
组分B: | |
Desmodur N 75(75%脂肪族异氰酸酯在乙酸甲氧基丙酯/二甲苯(1/)中) | 40.0 |
总和 | 140.0 |
将每种涂料配方喷射在白色涂覆铝面板(干膜厚:40μm)上,并在80℃下干燥30分钟以用于微生物测试。
实施例10:改性的AATCC-100
该测试方法是用于评估在纺织材料上的抗菌整理剂的AATCC标准100-1998的改进。该方法允许测试纺织材料以及硬表面的抗微生物活性。
向配有抗微生物涂层的硬表面接种确定细胞计数的特定检定菌。在适当的接种次数后,确定抗微生物整理的材料上的细胞计数,并与不含任何抗微生物剂的对照相比。
根据使用的需要,所述试样可以在适当的溶液如水、去离子水或7mMNaNO3中预接种。
每种抗微生物涂料接种两个样品。将每个样品放入灭菌的皮氏培养皿(55mm)中并接种适当量的细菌悬浮液(100μl-200μl),使得样品上的细菌最终浓度为~105cfu(菌落形成单位)。将接种的样品在恒湿室中在37℃下培养24小时。培养之后,向每个样品的皮氏培养皿中加入10ml灭活缓冲剂。摇晃该培养皿一分钟以收集存活菌后,得到在水中的稀释系列。将100μl未稀释的悬浮液以及1∶10和1∶1000的稀释液通过螺旋铺板器在具有灭活剂的胰蛋白大豆琼脂(Tryptic Soy Agar)上铺开。
然后将这些板在37℃下培养24-48小时(培养时间由所用细菌而定)。
经培养后,计算可见菌落,根据下式得到作为每个样品菌落形成单位[cfu/样品]的结果。
cfu/板×稀释因子×10×10
如果没有细菌菌落出现在未稀释悬浮液的板上,本方法的检测极限<100个细胞/样品。
通常在培养适当时间后,将具有抗微生物性质的样品上的细菌数[cfu/样品]与从未处理的的对照样品上洗脱的细胞计数进行比较。这两个值之间的区别提供了关于所测试材料的抗微生物整理剂或涂料的功效信息。
固体介质
酪蛋白-大豆粉蛋白胨-琼脂:
液体介质
培养基:
酪蛋白-大豆粉蛋白胨肉汤
灭活介质:
磷酸盐缓冲液0.07M,pH 7.4,含1%Tween 80和0.3%卵磷脂。
检定菌
大肠杆菌ATCC 10536
实施例8的紫外光透明涂料结果:
[cfu/样品]
样品 预培 在水中 在去离子 在7mM NaNO3
养前 预培养后 水中预培养后 中预培养后
不含银(对照) 3.0*106 1.0*105 1.8*107 4.7*105
2.8*106 4.5*105 1.5*107 5.6*105
0.5%带有载体 <100 8.5*105 1.5*107 9.5*105
的银*(比较) <100 1.7*106 9.2*106 9.4*105
0.5%带有载体 <100 <100 <100 <100
的银*/元素银**(发明) <100 <100 2.3*103 1.0*103
大肠杆菌ATCC 10536过夜培养物(O/n culture Escherichia coli ATCC 10536):2.2x109cfu/ml
**所用元素银是US-69984392的微米银。
实施例11:抗微生物液体硅橡胶(LSR)
将聚合物与本发明的添加剂在350°F(约177℃)下压缩成型10分钟,得到模制板(每个3×3英寸×125密耳;23克)。
为了进行比较,用同样方法制备仅仅含有元素银、仅仅含有带有载体的银、或完全不含银的对照配方。根据Bechert等的nature medicine 6,1053(2000)进行抗微生物活性评价;“起始OD[h]-净”的抗微生物阈值为6小时。所述样品在未进行预培养(表示短期功效)或者在预培养72h之后(7mM aq.NaNO3;模拟长期暴露于水)进行测试。
结果列于下表;评估:
+抗微生物活性,
-无抗微生物活性。
**所用元素银是US-6984392的微米银。
Claims (15)
1.一种抗微生物聚合物或涂料,所述聚合物或涂料包括有效抗微生物量的元素银和带有载体的银,其中所述带有载体的银负载于沸石或玻璃上。
2.根据权利要求1的抗微生物聚合物或涂料,其中所述带有载体的银负载于沸石上。
3.根据权利要求1的抗微生物聚合物或涂料,其中所述带有载体的银负载于玻璃上。
4.根据权利要求1的抗微生物聚合物或涂料,其中元素银/带有载体的银的基于银的重量/重量比为10∶1到1000∶1。
5.根据权利要求1的抗微生物聚合物或涂料,其中基于所述聚合物或涂料固体的重量,含有元素银0.01到5.0重量%,并且含有带有载体的银0.001到0.2重量%。
6.根据权利要求1的抗微生物聚合物或涂料,其中基于所述聚合物或涂料固体的重量,含有元素银大约0.01到2.0重量%,特别是0.01到1.0重量%,并且含有带有载体的银大约0.01到0.2重量%,特别是0.05到0.2重量%。
7.根据权利要求1的抗微生物聚合物或涂料,其中所述元素银以金属性微米粒子或纳米粒子存在。
8.根据权利要求1的抗微生物聚合物,其为纤维、膜、模制品或纺织或无纺织物。
9.根据权利要求1的抗微生物聚合物,其为聚氨酯、聚碳酸脂、液体硅橡胶、聚乙烯、聚丙烯、聚乙烯/聚丙烯共聚物或其为高分子复合材料。
10.根据权利要求1的抗微生物聚合物或涂料,其中所述元素银为微米级或纳米级。
11.根据权利要求1的抗微生物涂料。
12.根据权利要求1的抗微生物涂料,其为在塑料、木材、金属、陶瓷或塑木复合材料上的涂料。
13.根据权利要求1的抗微生物聚合物或涂料,其中还包含选自其他抗微生物剂、抗氧化剂、光稳定剂如紫外线吸收剂和/或立体受阻胺、亚磷酸盐、亚膦酸盐、成核剂、填料、增塑剂、颜料、阻燃剂、抗静电剂组成的组的一种或多种成分。
14.一种用于赋予聚合物或涂料以抗微生物活性的方法,包括向其中掺入有效抗微生物量的元素银和带有载体的银,其中所述带有载体的银负载于沸石或玻璃上。
15.元素银和带有载体的银的组合的用途,其中所述带有载体的银负载于沸石或玻璃上,用于赋予聚合物或涂料以抗微生物活性。
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- 2008-04-09 EP EP08736016.0A patent/EP2136645B1/en not_active Not-in-force
- 2008-04-09 AU AU2008240809A patent/AU2008240809B2/en not_active Ceased
- 2008-04-09 US US12/594,275 patent/US20100136073A1/en not_active Abandoned
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US10035131B2 (en) | 2011-11-24 | 2018-07-31 | Indian Institute Of Technology | Multilayer organic-templated-boehmite-nanoarchitecture for water purification |
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CN103747683A (zh) * | 2012-06-22 | 2014-04-23 | 印度理工学院 | 单容器重力进给储存水净化器 |
CN103747683B (zh) * | 2012-06-22 | 2017-02-15 | 印度理工学院 | 单容器重力进给储存水净化器 |
WO2015021757A1 (zh) * | 2013-08-10 | 2015-02-19 | 福建联迪商用设备有限公司 | 一种抗菌抗静电的金融pos机塑料外壳及其制备方法 |
CN106413557A (zh) * | 2014-05-22 | 2017-02-15 | 富士胶片株式会社 | 设备、保护片及抗菌膜 |
CN104447956A (zh) * | 2014-11-14 | 2015-03-25 | 陕西天瑞生物科技有限公司 | 聚氨酯界面特异性亲和多肽及其筛选方法 |
CN115397927A (zh) * | 2019-12-19 | 2022-11-25 | 奥贝蒂尔信托简易股份公司 | 特别用于安全文件的保护清漆 |
CN115427629A (zh) * | 2020-04-24 | 2022-12-02 | 赛杰法拉利股份有限公司 | 包含含银的硅酮表面层或氟化聚合物的复合膜,其生产方法及其作为抗病毒剂的用途 |
Also Published As
Publication number | Publication date |
---|---|
AU2008240809A1 (en) | 2008-10-30 |
JP2010525091A (ja) | 2010-07-22 |
CA2682509A1 (en) | 2008-10-30 |
CN101677575B (zh) | 2014-04-16 |
KR20100016595A (ko) | 2010-02-12 |
EP2136645A2 (en) | 2009-12-30 |
PL2136645T3 (pl) | 2013-11-29 |
ES2426216T3 (es) | 2013-10-22 |
AU2008240809B2 (en) | 2013-05-02 |
BRPI0810386A2 (pt) | 2014-11-25 |
JP5571548B2 (ja) | 2014-08-13 |
WO2008128896A3 (en) | 2009-01-22 |
WO2008128896A2 (en) | 2008-10-30 |
EP2136645B1 (en) | 2013-06-19 |
US20100136073A1 (en) | 2010-06-03 |
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