CN111344354B - 用于制备可焊接模制体的聚酰胺组合物 - Google Patents
用于制备可焊接模制体的聚酰胺组合物 Download PDFInfo
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- CN111344354B CN111344354B CN201880072372.1A CN201880072372A CN111344354B CN 111344354 B CN111344354 B CN 111344354B CN 201880072372 A CN201880072372 A CN 201880072372A CN 111344354 B CN111344354 B CN 111344354B
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- polyamide
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- copolyamide
- component
- polyamide composition
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- 239000004952 Polyamide Substances 0.000 title claims abstract description 124
- 229920002647 polyamide Polymers 0.000 title claims abstract description 124
- 239000000203 mixture Substances 0.000 title claims abstract description 118
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- 239000004953 Aliphatic polyamide Substances 0.000 claims abstract description 28
- 125000001931 aliphatic group Chemical group 0.000 claims abstract description 22
- 239000003365 glass fiber Substances 0.000 claims abstract description 18
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 14
- 229920000642 polymer Polymers 0.000 claims abstract description 14
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- -1 PA 5 Polymers 0.000 claims description 51
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- 238000000034 method Methods 0.000 claims description 25
- 238000002425 crystallisation Methods 0.000 claims description 20
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- PTJWCLYPVFJWMP-UHFFFAOYSA-N 2-[[3-hydroxy-2-[[3-hydroxy-2,2-bis(hydroxymethyl)propoxy]methyl]-2-(hydroxymethyl)propoxy]methyl]-2-(hydroxymethyl)propane-1,3-diol Chemical compound OCC(CO)(CO)COCC(CO)(CO)COCC(CO)(CO)CO PTJWCLYPVFJWMP-UHFFFAOYSA-N 0.000 claims description 5
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- 239000000835 fiber Substances 0.000 description 24
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- 239000012141 concentrate Substances 0.000 description 4
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- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- AOHJOMMDDJHIJH-UHFFFAOYSA-N propylenediamine Chemical compound CC(N)CN AOHJOMMDDJHIJH-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
- B29C65/02—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
- B29C65/02—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure
- B29C65/06—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure using friction, e.g. spin welding
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
- B29C65/02—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure
- B29C65/06—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure using friction, e.g. spin welding
- B29C65/0609—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure using friction, e.g. spin welding characterised by the movement of the parts to be joined
- B29C65/0618—Linear
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
- B29C65/02—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure
- B29C65/10—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure using hot gases (e.g. combustion gases) or flames coming in contact with at least one of the parts to be joined
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
- B29C65/02—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure
- B29C65/14—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure using wave energy, i.e. electromagnetic radiation, or particle radiation
- B29C65/16—Laser beams
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
- B29C65/82—Testing the joint
- B29C65/8207—Testing the joint by mechanical methods
- B29C65/8215—Tensile tests
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C66/00—General aspects of processes or apparatus for joining preformed parts
- B29C66/01—General aspects dealing with the joint area or with the area to be joined
- B29C66/05—Particular design of joint configurations
- B29C66/10—Particular design of joint configurations particular design of the joint cross-sections
- B29C66/11—Joint cross-sections comprising a single joint-segment, i.e. one of the parts to be joined comprising a single joint-segment in the joint cross-section
- B29C66/112—Single lapped joints
- B29C66/1122—Single lap to lap joints, i.e. overlap joints
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C66/00—General aspects of processes or apparatus for joining preformed parts
- B29C66/01—General aspects dealing with the joint area or with the area to be joined
- B29C66/05—Particular design of joint configurations
- B29C66/10—Particular design of joint configurations particular design of the joint cross-sections
- B29C66/12—Joint cross-sections combining only two joint-segments; Tongue and groove joints; Tenon and mortise joints; Stepped joint cross-sections
- B29C66/122—Joint cross-sections combining only two joint-segments, i.e. one of the parts to be joined comprising only two joint-segments in the joint cross-section
- B29C66/1222—Joint cross-sections combining only two joint-segments, i.e. one of the parts to be joined comprising only two joint-segments in the joint cross-section comprising at least a lapped joint-segment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C66/00—General aspects of processes or apparatus for joining preformed parts
- B29C66/40—General aspects of joining substantially flat articles, e.g. plates, sheets or web-like materials; Making flat seams in tubular or hollow articles; Joining single elements to substantially flat surfaces
- B29C66/41—Joining substantially flat articles ; Making flat seams in tubular or hollow articles
- B29C66/45—Joining of substantially the whole surface of the articles
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Abstract
本发明涉及聚酰胺组合物,其包含a)30至99.9重量%的聚酰胺混合物作为组分A),所述聚酰胺混合物为脂族聚酰胺A1)和脂族共聚酰胺或三聚酰胺A2)的混合物,A1)与A2)的重量比为55∶45至95∶5;b)0至60重量%的玻璃纤维作为组分B);c)0至2重量%的苯胺黑作为组分C);d)0.1至10重量%的至少一种具有多于两个羟基且数均分子量(Mn)小于2000的多羟基醇作为组分D);e)0至20重量%的其他添加剂作为组分E),所述组分量的总和相对于总的组合物而言为100重量%。
Description
本发明涉及适用于制备焊接成型制品的聚酰胺组合物、其制备方法及其用途,以及提高由聚酰胺组合物所制备的成型制品在热老化后的焊缝强度的方法。
聚酰胺是全球大规模生产的聚合物之一,其除了主要用于薄膜、纤维和成型制品(材料)的领域以外,还用于许多其他的终端用途。在聚酰胺中,聚酰胺-6(聚己内酰胺PA 6)和聚酰胺-6,6(尼龙,聚六亚甲基己二酰胺)是生产量最大的聚合物。大多数具有工业重要性的聚酰胺是以高的热稳定性为特征的半结晶热塑性聚合物。
由聚酰胺制成的成型制品可以通过焊接例如摩擦焊接、热气焊接或激光透射焊接来制备。
EP-B-1 060 216涉及一种用于可摩擦焊接成型制品的聚酰胺组合物,其中所述组合物(A)包含100重量份的(a)聚酰胺6和(b)脂族聚酰胺共聚物和/或脂族聚酰胺三元共聚物的聚酰胺混合物,其中(a)与(b)的重量比为95∶5至50∶50,以及(B)基于聚酰胺混合物的重量计10至100重量份的无机增强材料。还优选配合使用0.1至6重量份的增塑剂。所述增塑剂选自不含游离羟基或羧基的低分子量聚(乙二醇)酯和具有端羧基和端羟基的长链烷基聚酯。优选的增塑剂为2-乙基己酸封端的(N=9)聚(乙二醇)酯和长链烷基聚酯。所使用的共聚物为聚酰胺66/6共聚物或聚酰胺6/66/610三聚物。
还由WO 2010/014801已知耐热性聚酰胺成型制品的制备,其中使聚酰胺与以下多羟基醇混合:例如季戊四醇、二季戊四醇、三季戊四醇、二-三羟甲基丙烷、D-甘露糖醇、D-山梨糖醇或木糖醇。也可使用聚酰胺混合物。在示例性实施方案中,聚酰胺混合物包含占相对较大比例的至少半芳族的聚酰胺,以及占相对较小比例的脂族聚酰胺。
据说,由聚酰胺制备的成型制品,甚至在高温下经较长时间热老化后仍具有良好的机械性能。
DE-A-10 2017 100 932涉及作为粘合促进剂的羟基官能化树枝状聚合物。这些具有多个端羟基的树枝状聚合物尤其用作聚酰胺的粘合促进剂,以增加在粘合剂、特别是包含异氰酸酯基团的粘合剂的表面上的粘合力。
本发明的一个目的是提供适用于制备具有提高的热老化后焊缝强度的焊接成型制品的聚酰胺组合物。
根据本发明,该目的通过包含以下组分的聚酰胺组合物实现:
a)30重量%至99.9重量%的聚酰胺混合物作为组分A),其由脂族聚酰胺A1)和脂族共聚酰胺或三聚酰胺A2)组成,其中A1)与A2)的重量比为55∶45至95∶5;
b)0重量%至60重量%的玻璃纤维作为组分B);
c)0重量%至2重量%的苯胺黑作为组分C);
d)0.1重量%至10重量%的至少一种包含多于两个羟基且数均分子量(Mn)小于2000的多羟基醇作为组分D);
e)0重量%至20重量%的其他添加剂作为组分E),
其中所记录的量的总和100重量%是基于总的组合物计。
该目的还通过以下实现:制备聚酰胺组合物的方法,其通过在加热至温度为160℃至340℃时混合各成分而进行。
该目的还通过以下实现:聚酰胺组合物用于制备可焊接模制品或焊接成型制品的用途,以及通过由该聚酰胺组合物制成的可焊接模制品或焊接成型制品。
该目的还通过以下实现:具有多于两个羟基且数均分子量(Mn)小于2000的多羟基醇在含有至少一种聚酰胺和至少一种共聚酰胺或三聚酰胺的聚酰胺组合物中的用途,用于提高通过焊接由所述聚酰胺组合物而组成的至少两个模制品所制备的成型制品在热老化后的焊缝强度。
该目的还通过以下实现:提高成型制品在热老化后的焊缝强度的方法,所述成型制品由包含至少一种聚酰胺和至少一种共聚酰胺或三聚酰胺的聚酰胺组合物通过焊接至少两个模制品而制备,其中在制备模制品和成型制品之前,将聚酰胺组合物与基于总的聚酰胺组合物计0.1重量%至10重量%的至少一种具有多于两个羟基且数均分子量(Mn)小于2000的多羟基醇混合。
已发现,根据本发明,脂族聚酰胺A1)和脂族共聚酰胺或三聚酰胺A2)与组分D)的多羟基醇的结合所产生的聚酰胺组合物,可用于制备有益的焊接模制品,其中断裂伸长率或拉伸强度甚至是在高温下经长时间热处理(例如在180℃下热处理500小时)后仍能保持。
当使用(脂族)聚酰胺或(脂族)聚酰胺和共聚酰胺的聚酰胺混合物时,成型制品所获得的机械性能通常不足,并且由于热老化而进一步明显恶化。
多羟基醇在聚酰胺组合物中的使用通常会损害机械性能,特别是在焊接成型制品的情况下。这是由于醇对基础聚合物进行化学分解(降低粘度值),而短链醇在一定浓度和组合下还具有迁移的趋势。
只有通过将聚酰胺与共聚酰胺或三聚酰胺以及多羟基醇结合,才能获得具有良好的机械性能的聚酰胺组合物,所述机械性能即使在相对较长的热老化后也不会过度下降。另外,焊接成型制品在热老化之前和之后均显示出高的断裂伸长率。这些效果对于脂族聚酰胺与脂族共聚酰胺或三聚酰胺的结合物而言尤其明显。
由于苯胺黑会破坏并从而延缓结晶,所以苯胺黑的添加进一步改善机械性能。
本发明的聚酰胺组合物包含30重量%至99.9重量%、优选40重量%至99.5重量%、特别是50重量%至98.5重量%的组分A)。
它们还包含0重量%至60重量%、优选0重量%至40重量%、特别是0重量%至30重量%的组分B)。当存在组分B)时,最小量为优选5重量%、特别优选至少10重量%、特别是至少15重量%。由此得到组分B)的范围为5重量%至60重量%、优选10重量%至40重量%、特别优选15重量%至30重量%。
组分C)的用量为0重量%至2重量%、优选0重量%至1重量%、特别优选0重量%至0.5重量%。如果配合使用组分C),则下限优选为0.1重量%、特别优选0.15重量%、特别是0.2重量%。由此得到的用量范围为0.1重量%至2重量%、优选0.15重量%至1重量%、特别优选0.2重量%至0.5重量%。
组分D)的用量为0.1重量%至10重量%、优选0.5重量%至5重量%、特别是1.5重量%至3重量%。
组分E)的用量为0重量%至20重量%、优选0重量%至10重量%、特别是0重量%至5重量%。如果配合使用组分E),则下限优选为0.1重量%、特别优选至少0.2重量%、特别是至少0.3重量%。由此得到的范围为0.1重量%至20重量%、优选0.2重量%至10重量%、特别优选0.3重量%至5重量%、特别是0.3重量%至2重量%。
当存在组分B)、C)和/或E)时,组分A)的最大量随着各个组分的最小量和/或这些最小量之和相应地减少。当组分B)以5重量%的最小量存在时,组分A)的最大量例如因此降低至94.9重量%。
另外如果组分C)和E)各自以0.1重量%的最小量存在,则组分A)的最大量将因此而降低至94.7重量%。相应地处理其他用量范围,从而组分A)至E)的总量总是合计为100重量%。
本发明涉及基于脂族聚酰胺和共聚酰胺/三聚酰胺的特定的聚酰胺组合物。通常,本发明还涉及组分D)的多羟基醇在包含至少一种聚酰胺和至少一种共聚酰胺或三聚酰胺的聚酰胺组合物中的用途。适用于所述用途和所述方法的聚酰胺在下文中通常称为组分A)的合成聚酰胺。其对于聚酰胺和共聚酰胺/三聚酰胺进行了描述。在下文中,也描述了存在于聚酰胺组合物中的脂族(共)聚酰胺。
本发明的聚酰胺组合物包含至少一种合成聚酰胺作为组分A1和A2。在本发明的上下文中,术语“合成聚酰胺”应作广义地解释。通常,其包括含有至少一种适用于聚酰胺形成的组分的聚合物,并且所述组分选自二羧酸、二胺、至少一种二羧酸的盐和至少一种二胺的盐、内酰胺、ω-氨基酸、氨基腈及其混合物。除了适用于聚酰胺形成的组分外,本发明的合成聚酰胺还可包含可以共聚形式与其共聚的单体。术语“合成聚酰胺”不包括天然聚酰胺,例如肽和蛋白质,例如毛发、羊毛、丝绸和蛋白。
在本发明的上下文中,使用缩写来指代聚酰胺,其中一些缩写是本领域中惯用的,其由字母PA后加数字和字母组成。这些缩写中的一些已在DIN EN ISO 1043-1中标准化。可由H2N-(CH2)x-COOH类型的氨基羧酸或相应的内酰胺衍生的聚酰胺标识为PA Z,其中Z表示单体中的碳原子数。例如,PA 6代表ε-己内酰胺的聚合物或ω-氨基己酸的聚合物。可由H2N-(CH2)x-NH2和HOOC-(CH2)y-COOH类型的二胺和二羧酸衍生的聚酰胺标识为PA Z1Z2,其中Z1表示二胺中的碳原子数并且Z2表示二羧酸中的碳原子数。共聚酰胺通过按组分的比例顺序列出各组分并用斜线隔开来指定。例如,PA 66/610为六亚甲基二胺、己二酸和癸二酸的共聚酰胺。对于本发明所使用的具有芳族基团或脂环族基团的单体而言,使用以下字母缩写:
T=对苯二甲酸;I=间苯二甲酸;MXDA=间苯二甲胺;IPDA=异佛尔酮二胺;PACM=4,4′-亚甲基双(环己胺);MACM=2,2′-二甲基-4,4′-亚甲基双(环己胺)。
在下文中,表述“C1-C4-烷基”包含未取代的直链和支链的C1-C4-烷基基团。C1-C4-烷基基团的实例特别为甲基、乙基、丙基、异丙基、正丁基、异丁基、仲丁基、叔丁基(1,1-二甲基乙基)。
在下文中所述的脂族二羧酸、脂环族二羧酸、芳族二羧酸和一元羧酸的情况下,羧基可各自以未衍生化形式或以衍生物形式存在。在二羧酸的情况下,无羧基、一个羧基或两个羧基可为衍生物的形式。合适的衍生物为酸酐、酯、酰氯、腈和异氰酸酯。优选的衍生物为酸酐或酯。二羧酸的酸酐可为单体形式或聚合物形式。优选的酯为烷基酯和乙烯基酯,更优选C1-C4-烷基酯,特别是甲酯或乙酯。二羧酸优选为单烷基酯或二烷基酯的形式,更优选单C1-C4-烷基酯或二-C1-C4-烷基酯,特别是单甲酯、二甲酯、单乙酯或二乙酯。此外,二羧酸优选为单乙烯基酯或二乙烯基酯的形式。另外,二羧酸优选为混合酯的形式,更优选具有不同的C1-C4-烷基组成的混合酯,特别是甲基乙基酯。
适用于聚酰胺形成的组分优选选自:
pA)未取代或取代的芳族二羧酸和未取代或取代的芳族二羧酸的衍生物;
pB)未取代或取代的芳族二胺;
pC)脂族二羧酸或脂环族二羧酸;
pD)脂族二胺或脂环族二胺;
pE)一元羧酸;
pF)一元胺;
pG)至少三官能化胺;
pH)内酰胺;
pI)ω-氨基酸;
pK)不同于pA)至pI)且可与之共缩合的化合物。
一个合适的实施方案是脂族聚酰胺。对于PA Z1 Z2类型的脂族聚酰胺(例如PA66)而言,条件是必须存在组分pC)和pD)中的至少一种,并且组分pA)和pB)可均不存在。对于PA Z类型的脂族聚酰胺(例如PA 6或PA 12),条件是必须至少存在组分pH)。
另一个合适的实施方案是半芳族聚酰胺。对于半芳族聚酰胺而言,条件是必须存在组分pA)和pB)中的至少一种以及组分pC)和pD)中的至少一种。
芳族二羧酸pA)在每种情况下优选选自未取代或取代的邻苯二甲酸、对苯二甲酸、间苯二甲酸、萘二甲酸或联苯二甲酸,以及上述芳族二羧酸的衍生物和混合物。
取代的芳族二羧酸pA)优选具有至少一个(例如1、2、3或4个)C1-C4-烷基。特别地,取代的芳族二羧酸A)具有1个或2个C1-C4-烷基。这些优选选自甲基、乙基、正丙基、异丙基、正丁基、异丁基、仲丁基和叔丁基,更优选甲基、乙基和正丁基,特别是甲基和乙基并且尤其是甲基。取代的芳族二羧酸pA)也可带有不破坏酰胺化的其他官能团,例如5-磺酸基间苯二甲酸及其盐和衍生物。其优选的实例为5-磺酸基间苯二甲酸二甲酯的钠盐。
芳族二羧酸A)优选地选自未取代的对苯二甲酸、未取代的间苯二甲酸、未取代的萘二甲酸、2-氯对苯二甲酸、2-甲基对苯二甲酸、5-甲基间苯二甲酸和5-磺酸基间苯二甲酸。
特别优选所用的芳族二羧酸pA)为对苯二甲酸、间苯二甲酸或对苯二甲酸和间苯二甲酸的混合物。
含水溶液中的芳族二羧酸占全部的二羧酸的比例为至少50摩尔%、更优选70摩尔%至100摩尔%。在一个具体的实施方案中,所述半芳族聚酰胺中的对苯二甲酸或间苯二甲酸或对苯二甲酸和间苯二甲酸的混合物的比例,基于全部的二羧酸计,为至少50摩尔%、优选70摩尔%至100摩尔%。
芳族二胺pB)优选地选自双(4-氨基苯基)甲烷、3-甲基联苯胺、2,2-双(4-氨基苯基)丙烷、1,1-双(4-氨基苯基)环己烷、1,2-二氨基苯、1,4-二氨基苯、1,4-二氨基萘、1,5-二氨基萘、1,3-二氨基甲苯(类)、间苯二甲胺、N,N′-二甲基-4,4′-联苯二胺、双(4-甲基氨基苯基)甲烷、2,2-双(4-甲基氨基苯基)丙烷或其混合物。
脂族二羧酸或脂环族二羧酸pC)优选地选自乙二酸、丙二酸、丁二酸、戊二酸、己二酸、庚二酸、辛二酸、壬二酸、癸二酸、十一烷-α,ω-二羧酸、十二烷-α,ω-二羧酸、马来酸、富马酸或衣康酸、顺式环己烷-1,2-二羧酸和反式环己烷-1,2-二羧酸、顺式环己烷-1,3-二羧酸和反式环己烷-1,3-二羧酸、顺式环己烷-1,4-二羧酸和反式环己烷-1,4-二.羧酸、顺式环戊烷-1,2-二羧酸和反式环戊烷-1,2-二羧酸、顺式环戊烷-1,3-二羧酸和反式环戊烷-1,3-二羧酸及其混合物。
脂族二胺或脂环族二胺pD)优选地选自乙二胺、丙二胺、丁二胺、庚二胺、己二胺、戊二胺、辛二胺、壬二胺、癸二胺、十一烷二胺、十二烷二胺、2-甲基戊二胺、2,2,4-三甲基己二胺、2,4,4-三甲基己二胺、5-甲基壬二胺、2,4-二甲基辛二胺、5-甲基壬二胺、双(4-氨基环己基)甲烷、3,3′-二甲基-4,4′-二氨基二环己基甲烷及其混合物。
所述二胺D)更优选地选自己二胺、2-甲基戊二胺、辛二胺、壬二胺、2-甲基-1,8-辛二胺、癸二胺、十一烷二胺、十二烷二胺、双(4-氨基环己基)甲烷、3,3′-二甲基-4,4′-二氨基二环己基甲烷及其混合物。
在一个具体的实施方案中,所述半芳族聚酰胺包含至少一种选自以下的共聚二胺pD):己二胺、双(4-氨基环己基)甲烷(PACM)、3,3′-二甲基-4,4′-二氨基二环己基甲烷(MACM)、异佛尔酮二胺(IPDA)及其混合物。
在一个具体的实施方案中,所述半芳族聚酰胺仅包含己二胺作为共聚二胺pD)。
在另一个具体的实施方案中,所述半芳族聚酰胺仅包含双(4-氨基环己基)甲烷作为共聚二胺pD)。
在另一个具体的实施方案中,所述半芳族聚酰胺仅包含3,3′-二甲基-4,4′-二氨基二环己基甲烷(MACM)作为共聚二胺pD)。
在另一个具体的实施方案中,所述半芳族聚酰胺仅包含异佛尔酮二胺(IPDA)作为共聚二胺pD)。
所述脂族聚酰胺和半芳族聚酰胺可包含至少一种共聚一元羧酸pE)。所述一元羧酸pE)用于对根据本发明制备的聚酰胺进行封端。合适的一元羧酸原则上是所有的能够在聚酰胺缩合的反应条件下与至少一些可用的氨基反应的那些。合适的一元羧酸pE)为脂族一元羧酸、脂环族一元羧酸和芳族一元羧酸。这些包括乙酸、丙酸、正丁酸、异丁酸或叔丁酸、戊酸、三甲基乙酸、己酸、庚酸、辛酸、壬酸、癸酸、十一烷酸、十二烷酸、十三烷酸、肉豆蔻酸、棕榈酸、硬脂酸、新戊酸(pivalic acid)、环己烷甲酸、苯甲酸、甲基苯甲酸、α-萘甲酸、β-萘甲酸、苯乙酸、油酸、蓖麻油酸、亚油酸、亚麻酸、芥酸、脂肪酸(来自大豆、亚麻籽、蓖麻油植物和向日葵)、丙烯酸、甲基丙烯酸、酸、/>酸及其混合物。
如果所使用的一元羧酸pE)为不饱和羧酸或其衍生物,则在市售阻聚剂的存在下进行操作可能是有利的。
特别优选所述一元羧酸pE)选自乙酸、丙酸、苯甲酸及其混合物。
在一个具体的实施方案中,所述脂族聚酰胺和半芳族聚酰胺仅包含丙酸作为共聚一元羧酸pE)。
在另一个具体的实施方案中,所述脂族聚酰胺和半芳族聚酰胺仅包含苯甲酸作为共聚一元羧酸pE)。
在另一个具体的实施方案中,所述脂族聚酰胺和半芳族聚酰胺仅包含乙酸作为共聚一元羧酸pE)。
所述脂族聚酰胺和半芳族聚酰胺可包含至少一种共聚一元胺pF)。然后,所述脂族聚酰胺仅包含共聚脂族一元胺或脂环族一元胺。所述一元胺pF)用于对根据本发明制备的聚酰胺进行封端。合适的一元胺原则上是所有能够与在聚酰胺缩合的反应条件下与可用的羧酸基团的至少一部分反应的一元胺。合适的一元胺pF)为脂族一元胺、脂环族一元胺和芳族一元胺。这些包括甲胺、乙胺、丙胺、丁胺、己胺、庚胺、辛胺、癸胺、十八胺、二甲胺、二乙胺、二丙胺、二丁胺、环己胺、二环己胺、苯胺、甲苯胺、二苯胺、萘胺及其混合物。
可以额外地使用至少一种至少三价胺pG)以制备脂族聚酰胺和部分芳族聚酰胺。这些包括N′-(6-氨基己基)己烷-1,6-二胺、N′-(12-氨基十二烷基)十二烷-1,12-二胺、N′-(6-氨基己基)十二烷-1,12-二胺、N′-[3-(氨基甲基)-3,5,5-三甲基环己基]己烷-1,6-二胺、N′-[3-(氨基甲基)-3,5,5-三甲基环己基]十二烷-1,12-二胺、N′-[(5-氨基-1,3,3-三甲基环己基)甲基]己烷-1,6-二胺、N′-[(5-氨基-1,3,3-三甲基环己基)甲基]十二烷-1,12-二胺、3-[[[3-(氨基甲基)-3,5,5-三甲基环己基]氨基]甲基]-3,5,5-三甲基环己胺、3-[[(5-氨基-1,3,3-三甲基环己基)甲基氨基]甲基]-3,5,5-三甲基环己胺、3-(氨基甲基)-N-[3-(氨基甲基)-3,5,5-三甲基环己基]-3,5,5-三甲基环己胺。优选不使用至少三官能化胺pG)。
合适的内酰胺pH)为ε-己内酰胺、2-哌啶酮(δ-戊内酰胺)、2-吡咯烷酮(γ-丁内酰胺)、辛内酰胺(capryllactam)、庚内酰胺(enantholactam)、十二内酰胺(lauryllactam)及其混合物。
合适的ω-氨基酸pI)为6-氨基己酸、7-氨基庚酸、11-氨基十一烷酸、12-氨基十二烷酸及其混合物。
不同于pA)至pI)且可与之共缩合的合适的化合物pK)为至少三元羧酸、二氨基羧酸等。
合适的化合物pK)还包括4-[(Z)-N-(6-氨基己基)-C-羟基碳亚氨基(carbonimidoyl)]苯甲酸、3-[(Z)-N-(6-氨基己基)-C-羟基碳亚氨基]苯甲酸、(6Z)-6-(6-氨基己基亚氨基)-6-羟基己烷甲酸、4-[(Z)-N-[(5-氨基-1,3,3-三甲基环己基)甲基]-C-羟基碳亚氨基]苯甲酸、3-[(Z)-N-[(5-氨基-1,3,3-三甲基环己基)甲基]-C-羟基碳亚氨基]苯甲酸、4-[(Z)-N-[3-(氨基甲基)-3,5,5-三甲基环己基]-C-羟基碳亚氨基]苯甲酸、3-[(Z)-N-[3-(氨基甲基)-3,5,5-三甲基环己基]-C-羟基碳酰氨基]苯甲酸及其混合物。
所述聚酰胺优选地选自PA 4、PA 5、PA 6、PA 7、PA 8、PA 9、PA 10、PA 11、PA 12、PA 46、PA 66、PA 666、PA 69、PA 610、PA 612、PA 96、PA 99、PA 910、PA 912、PA 1212、PA6.T、PA 9.T、PA 8.T、PA 10.T、PA 12.T、PA 6.I、PA 8.I、PA 9.I、PA 10.I、PA 12.I、PA6.T/6、PA 6.T/10、PA 6.T/12、PA 6.T/6.I、PA 6.T/8.T、PA 6.T/9.T、PA 6.T/10T、PA 6.T/12.T、PA 12.T/6.T、PA 6.T/6.I/6、PA 6.T/6.I/12、PA 6.T/6.I/6.10、PA 6.T/6.I/6.12、PA 6.T/6.6、PA 6.T/6.10、PA 6.T/6.12、PA 10.T/6、PA 10.T/11、PA 10.T/12、PA 8.T/6.T、PA 8.T/66、PA 8.T/8.I、PA 8.T/8.6、PA 8.T/6.I、PA 10.T/6.T、PA 10.T/6.6、PA10.T/10.I、PA 10T/10.I/6.T、PA 10.T/6.I、PA 4.T/4.I/46、PA 4.T/4.I/6.6、PA 5.T/5.I、PA 5.T/5.I/5.6、PA 5.T/5.I/6.6、PA 6.T/6.I/6.6、PA MXDA.6、PA IPDA.I、PAIPDA.T、PA MACM.I、PA MACM.T、PA PACM.I、PA PACM.T、PA MXDA.I、PA MXDA.T、PA 6.T/IPDA.T、PA 6.T/MACM.T、PA 6.T/PACM.T、PA 6.T/MXDA.T、PA 6.T/6.I/8.T/8.I、PA 6.T/6.I/10.T/10.I、PA 6.T/6.I/IPDA.T/IPDA.I、PA6.T/6.I/MXDA.T/MXDA.I、PA 6.T/6.I/MACM.T/MACM.I、PA6.T/6.I/PACM.T/PACM.I、PA 6.T/10.T/IPDA.T、PA 6.T/12.T/IPDA.T、PA 6.T/10.T/PACM.T、PA 6.T/12.T/PACM.T、PA 10.T/IPDA.T、PA12.T/IPDA.T及其共聚物和混合物。
在一个优选的实施方案中,本发明的聚酰胺组合物包含至少一种脂族聚酰胺A1作为组分A)。
那么脂族聚酰胺优选地选自PA 4、PA 5、PA 6、PA 7、PA 8、PA 9、PA 10、PA 11、PA12、PA 46、PA 66、PA 666、PA 69、PA 610、PA 612、PA 96、PA 99、PA 910、PA 912、PA 1212及其共聚物和混合物。
所述脂族聚酰胺A1特别选自PA 6、PA 66或PA 12。一个具体的实施方案是聚酰胺组合物,其中所述组分A)包含PA 66或由PA 66组成。
半芳族聚酰胺/共聚酰胺优选地选自PA 6.T、PA 9.T、PA 10.T、PA12.T、PA 6.I、PA9.I、PA 10.I、PA 12.I、PA 6.T/6.I、PA 6.T/6、PA 6.T/8.T、PA 6.T/10T、PA 10.T/6.T、PA6.T/12.T、PA 12.T/6.T、PA IPDA.I、PA IPDA.T、PA 6.T/IPDA.T、PA 6.T/6.I/IPDA.T/IPDA.I、PA6.T/10.T/IPDA.T、PA 6.T/12.T/IPDA.T、PA 6.T/10.T/PACM.T、PA6.T/12.T/PACM.T、PA 10.T/IPDA.T、PA 12.T/IPDA.T及其共聚物和混合物。
在本发明的上下文中,随后的数均分子量Mn和重均分子量Mw是基于凝胶渗透色谱法(GPC)测定的。使用例如PMMA作为具有低的多分散性的聚合物标准品进行校准。
所述合成聚酰胺(例如A1或A2)的数均分子量Mn优选在8000至50000g/mol的范围内、更优选10000至35000g/mol。
所述合成聚酰胺(例如A1或A2)的数均分子量Mn优选在15000至200000g/mol范围内、更优选20000至125000g/mol。
所述聚酰胺(例如A1或A2)的多分散性PD(=Mw/Mn)优选不大于6、更优选不大于5、特别是不大于3.5。
相比之下,在本发明的聚酰胺组合物中,所述聚酰胺混合物A)包含脂族聚酰胺A1)和脂族共聚酰胺或三聚酰胺A2)。相应的组分可选自上文中所述的组分。
所述脂族聚酰胺A1)优选地选自:PA 4、PA 5、PA 6、PA 7、PA 8、PA 9、PA 10、PA11、PA 12、PA 46、PA 66、PA 69、PA 610、PA 612、PA 96、PA 99、PA 910、PA 912、PA 1212。
所述脂族聚酰胺A1)特别优选地选自聚酰胺6、聚酰胺66及其混合物。
所述脂族共聚酰胺或三聚酰胺A2优选由选自以下的两种或三种聚酰胺的单体构成:PA 4、PA 5、PA 6、PA 7、PA 8、PA 9、PA 10、PA 11、PA 12、PA 46、PA 66、PA 69、PA 610、PA 612、PA 96、PA 99、PA 910、PA 912、PA 1212。
共聚酰胺的具体实例为PA 66/6、PA 66/68、PA 66/610、PA 66/612、PA 66/10、PA66/12、PA 6/68、PA 6/610、PA 6/612、PA 6/10、PA 6/12。合适的三元共聚物的实例为PA 6/66/610、PA 6/66/69、PA 6/66/11、PA6/66/12、PA 6/610/11、PA 6/610/12、6/66/PACM。
所述脂族共聚酰胺优选为PA 6/PA 66共聚物。
合适的脂族聚酰胺和共聚酰胺/三聚酰胺还记载于EP-B-1060216中。
脂族聚酰胺A1)与脂族共聚酰胺或三聚酰胺A2)的重量比为55:45至95:5、优选60:40至90:10、特别是70:30至90:10。
所述聚酰胺混合物A)的结晶点(结晶温度)应优选低于所述脂族聚酰胺A1)和所述脂族共聚酰胺/三聚酰胺A2)的结晶点(结晶温度)。在本发明的用途和本发明的方法中,至少一种聚酰胺和至少一种共聚酰胺或三聚酰胺的混合物的结晶点也应优选低于所述至少一种聚酰胺和所述至少一种共聚酰胺或三聚酰胺的结晶点。
因此,优选地,加入的共聚酰胺/三聚酰胺具有使聚酰胺组合物的结晶点降低的作用。结晶点的下降或降低可通过DSC测量(差示扫描量热法)来测定。
通过将共聚酰胺/三聚酰胺与任选的苯胺黑添加物结合,可进一步降低聚酰胺组合物中的结晶温度。
本发明的聚酰胺组合物任选地包含玻璃纤维作为组分B)。当存在玻璃纤维时,组分A)的最大允许量随着玻璃纤维存在的最小量而减少。
具体而言,使用短切玻璃纤维。所述组分B)特别包含玻璃纤维,优选使用短纤维。这些短纤维优选长度在2至50mm且直径在5至40μm的范围内。或者,可以使用连续纤维(粗纱)。合适的纤维包括具有圆形和/或非圆形截面积的那些,其中在非圆形截面积的情况下,主截面轴与次截面轴的尺寸比特别是>2,优选2至8且特别优选3至5。
在一个具体的实施方案中,组分B)包含所谓的“扁平玻璃纤维”。具体地,这些纤维具有卵形或椭圆形的截面积或收缩的椭圆形(所谓的“茧”纤维)或矩形或近乎矩形的截面积。本文中优选使用的玻璃纤维具有非圆形截面积并且主截面轴与次截面轴的尺寸比例大于2、优选2至8、特别是3至5。
本发明的模塑材料的增强还可使用具有圆形和非圆形横截面的玻璃纤维的混合物来实现。在一个具体的实施方案中,如上所定义的扁平玻璃纤维的比例占主导地位,即它们占纤维总质量的50重量%以上。
当玻璃纤维的粗纱用作组分B)时,所述纤维优选具有直径为10至20μm、优选12至18μm。这些玻璃纤维的横截面可为圆形、卵形、椭圆形、近乎矩形或矩形。特别优选截面轴之比为2至5的所谓的扁平玻璃纤维。特别使用E玻璃纤维。但是,也可使用任何其他玻璃纤维类型,例如A、C、D、M、S或R玻璃纤维,或其任何所需的混合物或与E玻璃纤维的混合物。
本发明的聚酰胺模制材料可通过已知的制备长纤维增强的棒状粒料(pellet)的方法来制备,特别是通过拉挤成型法制备,其中连续的纤维束(粗纱)用聚合物熔体完全饱和,然后冷却和碎切。以这种方式获得的长纤维增强的棒状粒料(优选粒料长度为3至25mm、特别是4至12mm)可通过常规的加工方法(例如注射成型或加压成型)进一步进行加工以得到模制品。
本发明的聚酰胺组合物任选地包含苯胺黑作为组分C)。
苯胺黑(溶剂黑7-CAS:8005-02-5)为一种深黑色有机染料。
苯胺黑为合成的黑色着色剂的混合物,并且可通过在铁或铜催化剂的存在下加热硝基苯、苯胺和苯胺盐酸盐而获得。苯胺黑以各种形式存在(水溶性、醇溶性和油溶性)。典型的水溶性苯胺黑为酸性黑2(C.I.50420);典型的醇溶性苯胺黑为溶剂黑5(C.I.50415);典型的油溶性苯胺黑为溶剂黑7(C.I.50415:1)。
然而,就对健康可能造成的损害而言,苯胺黑并非完全无忧。例如,由于生产的结果,苯胺和硝基苯的残留物可能残留在产品中,并且在通过挤出方法、注塑方法或纺丝方法进行的后续加工过程中有形成不想要的分解产物的风险。
由于苯胺黑会破坏结晶,所以将苯胺黑添加到本发明的聚酰胺组合物中可进一步降低聚酰胺组合物的结晶倾向。该添加将引起更缓慢的结晶/降低结晶温度。
将至少一种具有多于两个羟基且数均分子量(Mn)小于2000的多羟基醇用作组分D)。所述多羟基醇记载于例如WO 2010/014801中,参见特别是其中的第14页第29行至第16页第7行。数均分子量优选通过凝胶渗透色谱法(GPC)测定。
所述多羟基醇可选自具有多于两个羟基的脂族羟基化合物、具有多于两个羟基的脂族-脂环族化合物、具有多于两个羟基的脂环族化合物、芳香族化合物和糖类。
多羟基醇中的脂族链不仅可以包含碳,而且可以包含杂原子,例如氮、氧或硫原子。多羟基醇中的脂环族环可为单环环体系或双环或多环环体系的一部分。其可以是碳环的或杂环的。所述多羟基醇可包含一个或多个取代基。例如醚、羧酸、羧酰胺或羧酸酯基团。
合适的多羟基醇的实例为三醇,例如丙三醇、三羟甲基丙烷、2,3-二-(2′-羟乙基)环己烷-1-醇、己烷-1,2,6-三醇、1,1,1-三(羟甲基)乙烷、3-(2′-羟基乙氧基)丙烷-1,2-二醇、3-(2′-羟基丙氧基)丙烷-1,2-二醇、2-(2′-羟基乙氧基)己烷-1,2-二醇、6-(2′-羟基丙氧基)己烷-1,2-二醇、1,1,1-三-[(2′-羟基乙氧基)甲基]乙烷、1,1,1-三-[(2′-羟基丙氧基)甲基]丙烷、1,1,1-三-(4′-羟基苯基)乙烷、1,1,1-三-(羟基苯基)丙烷、1,1,3-三-(二羟基-3-甲基苯基)丙烷、1,1,4-三(二羟基苯基)丁烷、1,1,5-三(羟基苯基)-3-甲基戊烷、二三羟甲基丙烷、三羟甲基丙烷乙氧基化物或三羟甲基丙烷丙氧基化物;多羟基醇,例如季戊四醇、二季戊四醇和三季戊四醇;以及糖类,例如环糊精、D-甘露糖、葡萄糖、半乳糖、蔗糖、果糖、木糖、阿拉伯糖、D-甘露糖醇、D-山梨糖醇、D-阿拉伯糖醇或L-阿拉伯糖醇、木糖醇、艾杜糖醇(iditol)、塔罗糖醇(talitol)、蒜糖醇(allitol)、阿卓糖醇(altritol)、guilitol、赤藓糖醇(erythritol)、苏糖醇(threitol)和D-古洛糖酸-γ-内酯(D-gulono-γ-lactone)。
在优选的多羟基醇中,所述羟基各自与彼此被至少一个原子(优选一个碳原子)隔开的碳原子键合。因此,所述多羟基醇优选为季戊四醇、二季戊四醇、三季戊四醇、三羟甲基丙烷、D-甘露糖醇、D-山梨糖醇或木糖醇。特别优选所述多羟基醇为二季戊四醇和/或三季戊四醇。最优选二季戊四醇。
所述聚酰胺组合物可包含其他添加剂作为组分E)。如果配合使用组分E),则组分A)的上限相应地降低。
作为组分E),本发明的组合物包含0重量%至20重量%、优选0重量%至10重量%且特别是0重量%至5重量%的其他添加剂。如果配合使用所述添加剂,则最小量为0.1重量%、优选1重量%、特别是3重量%。
如果配合使用组分E),则组分A)的上限相应地降低。因此在组分E)的最小量为0.1重量%时,组分A)的量的上限为例如约89.8重量%。
所考虑的其他添加剂包括不同于玻璃纤维的填料和增强材料、不同于组分A的热塑性聚合物或其他添加剂。
在本发明的上下文中,术语“填料和增强材料”(=可能的组分E))应作广义地解释并且包含颗粒状填料、纤维状物质和任何的中间形式。颗粒状填料可具有很宽的粒径范围,从粉尘形式的颗粒到大颗粒。所考虑的填料材料包括有机填料或无机填料和增强材料。本文中可使用的为例如无机填料,例如高岭土、白垩、硅灰石、滑石、碳酸钙、硅酸盐、二氧化钛、氧化锌、石墨、玻璃颗粒(例如玻璃球)、纳米级填料(例如碳纳米管)、纳米级片状硅酸盐、纳米级氧化铝(Al2O3)、纳米级二氧化钛(TiO2)、石墨烯、永久磁性或可磁化金属化合物和/或合金、层状硅酸盐和纳米级二氧化硅(SiO2)。所述填料也可能已经经过表面处理。
可用于本发明的模制材料中的层状硅酸盐的实例包括高岭土、蛇纹石、滑石、云母、蛭石、伊利石、蒙皂石、蒙脱石、锂蒙脱石、双氢氧化物或其混合物。所述层状硅酸盐可能已经经过表面处理或未处理。
还可使用一种或多种纤维状物质。这些纤维状物质优选选自已知的无机增强纤维,例如硼纤维、碳纤维、二氧化硅纤维、陶瓷纤维和玄武岩纤维;有机增强纤维,例如芳纶纤维、聚酯纤维、尼龙纤维、聚乙烯纤维;和天然纤维,例如木纤维、亚麻纤维、大麻纤维和剑麻纤维。
特别优选使用碳纤维、芳纶纤维、硼纤维、金属纤维或钛酸钾纤维。
不同于组分A)的热塑性聚合物优选地选自:
-均聚物或共聚物,其包含呈共聚形式的至少一种选自C2-C10-单烯烃的单体例如乙烯或丙烯、1,3-丁二烯、2-氯-1,3-丁二烯、乙烯醇及其C2-C10-烷基酯、氯乙烯、偏二氯乙烯、偏二氟乙烯、四氟乙烯、丙烯酸缩水甘油酯、甲基丙烯酸缩水甘油酯、具有支链和直链C1-C10-醇的醇组分的丙烯酸酯和甲基丙烯酸酯、乙烯基芳族化合物(例如苯乙烯)、丙烯腈、甲基丙烯腈、α,β-烯键式不饱和一元羧酸和二元羧酸以及马来酸酐;
-乙烯基缩醛的均聚物和共聚物;
-聚乙烯酯;
-聚乙烯吡咯烷酮或聚乙烯吡咯烷酮共聚物(PVP);
-聚碳酸酯(PC);
-聚酯,例如聚对苯二甲酸亚烷基酯、聚羟基脂肪酸酯(PHA)、聚丁二酸丁二醇酯(PBS)、聚丁二酸己二酸丁二醇酯(PBSA);
-聚醚;
-聚醚酮;
-热塑性聚氨酯(TPU);
-聚硫化物;
-聚砜;
-聚醚砜;
-纤维素烷基酯
及其混合物。
实例包括来自C4-C8醇(特别是丁醇、己醇、辛醇和2-乙基己醇)中的相同或不同的醇基团的聚丙烯酸酯、聚甲基丙烯酸甲酯(PMMA)、甲基丙烯酸甲酯-丙烯酸丁酯共聚物、丙烯腈-丁二烯-苯乙烯共聚物(ABS)、乙烯-丙烯共聚物、乙烯-丙烯-二烯共聚物(EPDM)、聚苯乙烯(PS)、苯乙烯-丙烯腈共聚物(SAN)、丙烯腈-苯乙烯-丙烯酸酯(ASA)、苯乙烯-丁二烯-甲基丙烯酸甲酯共聚物(SBMMA)、苯乙烯-马来酸酐共聚物、苯乙烯-甲基丙烯酸共聚物(SMA)、聚甲醛(POM)、聚乙烯醇(PVAL)、聚乙酸乙烯酯(PVA)、聚乙烯醇缩丁醛(PVB)、聚己内酯(PCL)、聚羟基丁酸(PHB)、聚羟基戊酸(PHV)、聚乳酸(PLA)、乙基纤维素(EC)、乙酸纤维素(CA)、丙酸纤维素(CP)或乙酸/丁酸纤维素(CAB)。
存在于本发明的模塑材料中的至少一种热塑性聚合物优选为聚氯乙烯(PVC)、聚乙烯醇缩丁醛(PVB)、乙酸乙烯酯的均聚物和共聚物、苯乙烯的均聚物和共聚物、聚丙烯酸酯、热塑性聚氨酯(TPUs)或聚硫化物。
使用任选地与至少一种其他着色剂结合的溶剂黑28(CAS号12237-23-91)可能是有利的。于是组分E)优选地选自不同于C)的非成核着色剂。这些包括非成核染料、非成核颜料及其混合物。非成核染料的实例为溶剂黄21(可从BASF SE以Yellow 160FA商购获得)或溶剂蓝104(可从Clariant以/>Blue 2B商购获得)。非成核颜料的实例为颜料棕24(可从BASF SE以/>Yellow K 2011FG商购获得)。少量的至少一种白色颜料也可用作组分E)。合适的白色颜料为二氧化钛(颜料白6)、硫酸钡(颜料白22)、硫化锌(颜料白7)等。在一个具体的实施方案中,本发明的模制材料包含0.001重量%至0.5重量%的至少一种白色颜料作为组分E)。例如,所述模制材料可包含0.05重量%的来自Kronos的Kronos 2220二氧化钛。
添加的方式和量由色相,即所需的黑色深浅所决定。例如,对于溶剂黄21,可在CIELAB颜色空间中将黑色色相从例如b*=-1.0沿+b*方向(即沿黄色方向)移动。对于本领域技术人员而言该方法称为色差法。根据DIN 6174《根据近似均匀CIELAB颜色空间的比色评估色彩坐标和色差(Colorimetric evaluation of colour coordinates and colourdifferences according to the approximately uniform CIELAB colour space)》或后续标准进行测量。
还可配合使用炭黑作为组分E)。本发明的组合物包含例如0.01重量%至1重量%、优选0.03重量%至0.5重量%、特别是0.05重量%至0.3重量%的炭黑。炭黑(也称为工业炭黑)是一种具有高的表面-体积比的改性碳,并且由80重量%至99.5重量%的碳组成。炭黑的比表面积为约10至1500m2/g(BET)。所述炭黑已经以槽法炭黑、炉黑、焰黑、裂化黑或乙炔黑的形式制备。颗粒直径的范围为8至500nm,通常为8至110nm。炭黑也称为颜料黑7或灯黑6。着色用炭黑(color black)为纳米颗粒状炭黑,由于其细度而逐渐失去了常规炭黑的棕色基础色。
合适的优选添加剂E)为润滑剂和热稳定剂,而且还为阻燃剂、光稳定剂(UV稳定剂、UV吸收剂或UV阻断剂)、染料、成核剂、金属颜料、金属薄片、金属涂覆的颗粒、抗静电剂、导电添加剂、脱模剂、荧光增白剂、消泡剂等。
作为组分E),本发明的模制材料可包含优选0.01重量%至3重量%、特别优选0.02重量%至2重量%、特别是0.05重量%至1.0重量%的至少一种热稳定剂,基于组合物的总重量计。
所述热稳定剂优选选自铜化合物、仲芳族胺、位阻酚、亚磷酸酯、亚膦酸酯及其混合物。
如果使用铜化合物,则铜的量为优选0.003重量%至0.5重量%、特别是0.005重量%至0.3重量%且特别优选0.01重量%至0.2重量%,基于组合物的总重量计。
如果使用基于仲芳族胺的稳定剂,则这些稳定剂的量为优选0.2重量%至2重量%、特别优选0.2重量%至1.5重量%,基于组合物的总重量计。
如果使用基于位阻酚的稳定剂,则这些稳定剂的量为优选0.1重量%至1.5重量%、特别优选0.2重量%至1重量%,基于组合物的总重量计。
如果使用基于亚磷酸酯和/或亚膦酸酯的稳定剂,则这些稳定剂的量为优选0.1重量%至1.5重量%、特别优选0.2重量%至1重量%,基于组合物的总重量计。
合适的一价铜或二价铜的化合物E)为例如一价铜或二价铜与无机酸或有机酸或一元酚或二元酚的盐、一价铜或二价铜的氧化物或铜盐与氨、胺、酰胺、内酰胺、氰化物或膦的配合物,优选氢卤酸的Cu(I)或Cu(II)盐或氢氰酸的Cu(I)或Cu(II)盐或脂族羧酸的铜盐。特别优选一价铜化合物CuCl、CuBr、CuI、CuCN和Cu2O,以及二价铜化合物CuCl2、CuSO4、CuO、乙酸铜(II)或硬脂酸铜(II)。
所述铜化合物是可商购获得的和/或其制备是本领域技术人员已知的。所述铜化合物可以原样使用或以浓缩物形式使用。浓缩物应理解为意指优选具有与组分A)相同的化学性质的包含高浓度铜盐的聚合物。浓缩物的使用是常规方法,并且尤其是在需要添加非常少量的原料时,常常使用浓缩液。这是有利的,将铜化合物与其他金属卤化物,特别是碱金属卤化物(例如NaI、KI、NaBr、KBr)结合使用,其中金属卤化物与铜卤化物的摩尔比为0.5至20、优选1至10且特别优选3至7。
本发明基于仲芳族胺且可用的稳定剂的特别优选的实例包括苯二胺与丙酮的加合物(A)、苯二胺与亚麻酸的加合物、4,4′-双(α,α-二甲基苄基)二苯胺(/>445)、N,N′-二萘基对苯二胺、N-苯基-N′-环己基对苯二胺或其两种或更多种的混合物。
本发明可使用的且基于位阻酚的稳定剂的优选实例包括N,N′-六亚甲基双-3-(3,5-二叔丁基-4-羟基苯基)丙酰胺、双(3,3-双(4′-羟基-3′-叔丁基苯基)丁酸)乙二醇酯、2,1′-硫代乙基双(3-(3,5-二叔丁基-4-羟基苯基))丙酸酯、4,4′-亚丁基双(3-甲基-6-叔丁基苯酚)、三乙二醇3-(3-叔丁基-4-羟基-5-甲基苯基)丙酸酯或这些稳定剂的两种或更多种的混合物。
优选的亚磷酸酯和亚膦酸酯为亚磷酸三苯酯、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、二亚磷酸二硬脂基季戊四醇酯、亚磷酸三(2,4-二叔丁基苯基)酯、二亚磷酸二异癸基季戊四醇酯、二亚磷酸双(2,4-二叔丁基苯基)季戊四醇酯、二亚磷酸双(2,6-二叔丁基-4-甲基苯基)季戊四醇酯、二亚磷酸二异癸氧基季戊四醇酯、二亚磷酸双(2,4-二叔丁基-6-甲基苯基)季戊四醇酯、二亚磷酸双(2,4,6-三(叔丁基苯基))季戊四醇酯、三硬脂基山梨糖醇三亚磷酸酯、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]-1,3,2-二氧杂膦(dioxaphosphocin)、6-氟-2,4,8,10-四叔丁基-12-甲基二苯并-[d,g]-1,3,2-二氧杂膦、亚磷酸双(2,4-二叔丁基-6-甲基苯基)甲酯和亚磷酸双(2,4-二叔丁基-6-甲基苯基)乙酯。特别优选亚磷酸三[2-叔丁基-4-硫代(2′-甲基-4′-羟基-5′-叔丁基)苯基-5-甲基]苯基酯和亚磷酸三(2,4-二叔丁基苯基)酯(PAR24:可从BASF SE商购获得)。
热稳定剂的一个优选的实施方案包括有机热稳定剂(特别是PAR 24和/>1010)、基于双酚A的环氧化物(特别是/>1001)和基于CuI和KI的铜稳定剂的组合。可商购获得的由有机稳定剂和环氧化物组成的稳定剂混合物的实例为购自BASF SE的/>NC66。特别优选仅基于CuI和KI的热稳定剂。除了添加铜或铜化合物外,还排除使用其他过渡金属化合物,特别是元素周期表中VB、VIB、VIIB或VIIIB族的金属盐或金属氧化物。另外,优选不向本发明的模制材料中添加元素周期表中VB、VIB、VIIB或VIIIB族的任何过渡金属,例如铁粉或钢粉。
本发明的模制材料包含,基于组合物的总重量计,0重量%至15重量%、特别优选0重量%至10重量%的至少一种阻燃剂作为添加剂E)。当本发明的模制材料包含至少一种阻燃剂时,则其量优选为0.01至15重量%、特别优选0.1至10重量%,基于组合物的总重量计。合适的阻燃剂包括含卤素和无卤素阻燃剂及其增效剂(另请参见第3版1989Hanser Verlag,第11章)。优选的无卤素阻燃剂为红磷、次膦酸盐或二次膦酸盐和/或含氮阻燃剂,例如三聚氰胺、三聚氰胺氰尿酸盐、三聚氰胺硫酸盐、三聚氰胺硼酸盐、三聚氰胺草酸盐、三聚氰胺磷酸盐(伯、仲)或仲三聚氰胺焦磷酸盐、新戊二醇硼酸三聚氰胺、胍及本领域技术人员已知的其衍生物,以及聚合三聚氰胺磷酸盐(CAS号:56386-64-2和218768-84-4以及EP-A-1095030)、多磷酸铵、三羟乙基异氰脲酸酯(也任选多磷酸铵与三羟乙基异氰脲酸酯的混合物)(EP-A-0584567)。其他含N或含P的阻燃剂或适合作为阻燃剂的PN缩合物,以及其常规的增效剂(例如氧化物或硼酸盐)可见于DE-A-102004049342中。合适的卤化阻燃剂为例如低聚溴化聚碳酸酯(BC 52Great Lakes)或N大于4的聚五溴苄基丙烯酸酯(FR1025Dead sea bromine)、四溴双酚A与环氧化物的反应产物、溴化低聚苯乙烯或溴化聚合苯乙烯、得克隆(dechlorane),所述卤化阻燃剂通常与氧化锑一起用作增效剂(有关详情及其他阻燃剂请参见DE-A-102004050025)。
所述聚酰胺模制材料通过本身已知的方法制备。这些方法包括使组分以适当的重量比例混合。组分的混合优选在高温下通过混合、共混、捏合、挤出或辊压来完成。混合期间的温度为优选220℃至340℃、特别优选240℃至320℃且特别是250℃至300℃。合适的方法是本领域技术人员已知的。
模制品/成型制品
本发明还涉及使用本发明的聚酰胺模制材料制备的模制品和成型制品。
成型制品由多个(即两个或更多个)模制品特别通过焊接构成。
所述聚酰胺模制材料可以通过任何所需的合适的加工技术来制备模制品和成型制品。合适的加工技术特别是注射成型、挤出、共挤出、热成型或任何其他已知的聚合物成型方法。这些和其他实例可见于例如″von Kunststoffen″[Coloring ofPlastics],VDI-Verlag,ISBN3-18-404014-3中。
通过本发明的方法可获得的聚酰胺模制材料还有利地适合用于汽车应用、用于尤其是包括在高温部分中的电气和电子部件的模制品的生产。
一个具体的实施方案是以部件形式或作为部件的一部分用于汽车领域的模制品或成型制品,所述汽车领域特别选自汽缸盖罩、发动机罩、用于增压空气冷却器的外壳、增压空气冷却器阀、进气口管道、进气歧管、连接器、齿轮、风扇叶轮、冷却水箱、热交换器的外壳或外壳零件、冷却剂冷却器、增压空气冷却器、恒温器、水泵、加热元件、固定零件。
汽车内饰的可能用途是用于仪表板、转向柱开关、座椅部件、头枕、中控台、变速箱部件和门组件;以及汽车外饰的可能用途是用于A、B、C或D立柱罩、扰流板、门把手、外后视镜部件、雨刷部件、雨刷防护罩、装饰格栅、盖条、顶部桁材、窗框、天窗框架、天线罩、前灯和尾灯、发动机罩、汽缸盖罩、进气口管道、雨刷和车身外部零件。
另一具体的实施方案是以其本身或作为电气或电子无源或有源组件、印刷电路板、部分印刷电路板、外壳组成、膜或电线的一部分的模制品或成型制品,尤其是以下述形式或作为下述一部分:开关、插头、套管、分配器、继电器、电阻器、电容器、绕组或绕组体、灯、二极管、LED、晶体管、连接器、调节器、集成电路(IC)、处理器、控制器、存储元件和/或传感器。
本发明的聚酰胺在厨房和家用领域的可能用途是用于生产厨房机器(例如油炸锅、熨斗、旋钮)的部件以及在园林和休闲领域的应用(例如用于灌溉系统或园林设备和门把手的部件)。
用于制备模制品的聚酰胺组合物通过本身已知的方法制备。本文中参考上述用于制备聚酰胺组合物的方法。这些方法包括以适当的重量比例混合组分。组分的混合优选在高温下通过混合、共混、捏合、挤出或辊压来完成。混合期间的温度为优选220℃至340℃、特别优选240℃至320℃且特别是250℃至300℃。各个组分的预混合可能是有利的。还可进一步由预混合组分和/或单个组分的物理混合物(干混料)直接制备模制品,所述物理混合物已在远低于所述聚酰胺的熔点下制备。在这种情况下,混合期间的温度为优选0℃至100℃、特别优选10℃至50℃、特别是环境温度(25℃)。可通过常规方法(例如通过注塑或挤出)将所述模制材料加工成模制品。所述材料特别适合于例如用于盖、外壳、配件、传感器的材料;用于例如在汽车、电气工程、电子、电信、信息技术、计算机、家用、体育、医疗或娱乐领域中。
本发明的聚酰胺组合物特别适用于制备可焊接模制品和焊接模制品(将可焊接模制品通过焊接制得)。所述(焊接)成型制品在焊接后显示出良好的机械性能。特别是在180℃下热老化2000小时后,所述焊接成型制品的拉伸强度或断裂应力得以很大程度地保持。在180℃下热处理500小时后,所述焊接成型制品的拉伸强度或断裂应力仅略有下降。因此,热老化以类似于汽车工业中常用的规格进行。
因此,使用本发明的模制材料,特别是配合使用共聚酰胺/三聚酰胺和任选地苯胺黑与多羟基醇,在最初和老化后均可以显著改善焊缝。因此,可以克服记载于WO 2010/014801和EP-B-1 060 216中的模制材料在相关应用中的缺点。由聚酰胺组合物通过焊接至少两个模制品而制备的成型制品在氧化和热老化之前和之后均显示出改善的焊缝强度。
所述成型制品的焊接可通过任何所需的焊接方法进行,例如通过摩擦焊接、热气焊接或通过束焊接(例如激光透射焊接)进行。相应的焊接方法是本领域技术人员已知的,并且记载于例如WO 2013/139802中。
下文中通过以下实施例对本发明进行更具体地阐述。
使用以下原料:
A/1:聚酰胺6:来自BASF SE的B27,熔点:222℃,粘度值(0.5%,于96%H2SO4中):150cm3/g聚酰胺的粘度值根据ISO 307在25℃下进行测定。
A/2:聚酰胺6/聚酰胺66共聚物,来自BASF SE的C27,熔点:195℃至197℃,粘度值(0.5%,于96%H2SO4中):145cm3/g
聚酰胺的粘度值根据ISO 307在25℃下进行测定。
B:玻璃纤维:NEG-T249H,制造商:Nippon Electric Glass(Mal aysia)SDN.BHD.,平均直径:10.5μm,长度:3mm
C:苯胺黑/溶剂黑7,制造商:Colloids Ltd.
D/1:热稳定剂:CuI/KI,摩尔比为1∶4
D/2:二季戊四醇(CAS:126-58-9)
E:润滑剂:EBS,制造商:Lonza Cologne GmbH,
亚乙基双(硬脂酰胺)(二硬脂基亚乙基二酰胺)CAS号110-30-5
将下表1中列出的成分在滚筒式混合器中预混合10分钟,然后在300℃的滚筒温度下通过直径为25mm且L/D比为44的双螺杆挤出机挤出并造粒。为此,首先将天然色聚酰胺粒料在干燥箱中在100℃下干燥4小时,以使水分含量低于0.1%。将所得的粒料在300℃熔融温度下、在注塑机上注射成型,得到厚度为2mm且尺寸为60x 60mm的饰板,并通过目测和分析来评估。机械性能根据DIN ISO 527或179-2/1eU或179-2/1eAf(2017版)进行测定。
如下所述进行焊接成型制品的制备。为此,通过注射成型制备尺寸为(110x 110x4)mm3的饰板。如图1所示,将饰板从中心处分开,并在偏移后进行焊接。由焊接饰板来制备具有对应的中心焊缝的拉伸试样。丢弃外围区域。使用Branson Type-M-102H机器(~240Hz)进行振动焊接,参数如下:
使用Zwick Type 1446拉力试验机(10mm/min,室温)进行拉伸试验。
按照常规汽车标准进行热老化。为此,将再循环烘箱进行温度控制至正确的温度。在各个步骤之前,将试样在负压下在80℃的温度下干燥48小时。随后将它们在温度控制的烘箱中存储给定的时间。
图1示意性地示出,在左上方处使注射成型的饰板分开、在右上方处将这两部分焊接以及在底部,使焊接饰板分开以获得试验样品1、2和3。丢弃阴影的外围区域。
表1
比较实施例C1描述了用于汽车领域的传统配方。比较实施例C2示出共聚酰胺的配合使用。在这两种情况下,焊接成型制品在热老化后的断裂伸长率均是不充分的。
比较实施例C3涉及多羟基醇在聚酰胺模塑材料中的用途。焊接成型制品的断裂伸长率是不充分的。只有通过在模塑材料中将共聚酰胺与多羟基醇结合,才实现焊接成型制品在热老化之前和之后足够的断裂应力。
Claims (12)
1.聚酰胺组合物,其包含:
a)30重量%至99.9重量%的聚酰胺混合物作为组分A),其由脂族聚酰胺A1)和脂族共聚酰胺A2)组成,其中A1)与A2)的重量比为55:45至95:5,
b)0重量%至60重量%的玻璃纤维作为组分B),
c)0重量%至2重量%的苯胺黑作为组分C),
d)0.1重量%至10重量%的至少一种包含多于两个羟基且数均分子量(Mn)小于2000的多羟基醇作为组分D),所述组分
D)为季戊四醇、二季戊四醇和/或三季戊四醇,
e)0重量%至20重量%的其他添加剂作为组分E),
其中所记录的量的总和为100重量%,基于总的组合物计;
所述脂族聚酰胺A1)选自PA 4、PA 5、PA 6、PA 7、PA 8、PA 9、PA 10、PA 11、PA 12、PA46、PA 66、PA 69、PA 610、PA 612、PA 96、PA 99、PA 910、PA 912、PA 1212;并且所述脂族共聚酰胺A2)是PA 4、PA 5、PA 6、PA 7、PA 8、PA 9、PA 10、PA 11、PA 12、PA 46、PA 66、PA 69、PA 610、PA 612、PA 96、PA 99、PA 910、PA 912和PA 1212中两种或三种的共聚酰胺。
2.根据权利要求1所述的聚酰胺组合物,其中所述脂族聚酰胺A1)选自PA 6、PA66及其混合物。
3.根据权利要求1或2所述的聚酰胺组合物,其中所述脂族共聚酰胺A2)为PA6/PA66共聚物。
4.根据权利要求1或2所述的聚酰胺组合物,其中存在0.1重量%至2重量%的苯胺黑作为组分C)。
5.根据权利要求1或2所述的聚酰胺组合物,其中在所述聚酰胺组合物中至少一种聚酰胺和至少一种共聚酰胺的混合物的结晶点低于所述至少一种聚酰胺和至少一种共聚酰胺的结晶点。
6.一种制备根据权利要求1至5中任一项所述的聚酰胺组合物的方法,其通过在加热至温度160℃至340℃下,混合各成分而制备。
7.根据权利要求1至5中任一项所述的聚酰胺组合物用于制备可焊接模制品或焊接成型制品的用途。
8.一种可焊接模制品或焊接成型制品,其由根据权利要求1至5中任一项所述的聚酰胺组合物组成。
9.具有多于两个羟基且数均分子量(Mn)小于2000的多羟基醇在包含至少一种聚酰胺和至少一种共聚酰胺的聚酰胺组合物中的用途,用于提高通过焊接至少两个由所述聚酰胺组合物组成的模制品所制备的成型制品在热老化后的焊缝强度;所述至少一种聚酰胺选自PA4、PA 5、PA6、PA7、PA8、PA9、PA10、PA11、PA 12、PA46、PA 66、PA 69、PA 610、PA 612、PA 96、PA 99、PA 910、PA 912、PA 1212;并且所述至少一种共聚酰胺是PA 4、PA 5、PA 6、PA 7、PA8、PA 9、PA 10、PA 11、PA 12、PA 46、PA 66、PA 69、PA 610、PA 612、PA 96、PA 99、PA 910、PA 912和PA 1212中两种或三种的共聚酰胺;
其中所述聚酰胺组合物如权利要求1至5中任一项所定义地构成。
10.根据权利要求9所述的用途,其中在所述聚酰胺组合物中至少一种聚酰胺和至少一种共聚酰胺的混合物的结晶点低于所述至少一种聚酰胺和至少一种共聚酰胺的结晶点。
11.一种提高成型制品在热老化后的焊缝强度的方法,所述成型制品由包含至少一种聚酰胺和至少一种共聚酰胺的聚酰胺组合物,通过焊接至少两个模制品而制备,其中在制备所述模制品和所述成型制品之前,将所述聚酰胺组合物与基于总的聚酰胺组合物计0.1重量%至10重量%的至少一种具有多于两个羟基且数均分子量(Mn)小于2000的多羟基醇混合;所述至少一种聚酰胺选自PA 4、PA 5、PA 6、PA 7、PA 8、PA 9、PA 10、PA 11、PA 12、PA46、PA 66、PA 69、PA 610、PA 612、PA 96、PA 99、PA 910、PA 912、PA 1212;所述至少一种共聚酰胺是PA 4、PA 5、PA 6、PA 7、PA 8、PA 9、PA 10、PA 11、PA 12、PA 46、PA 66、PA 69、PA610、PA 612、PA 96、PA 99、PA 910、PA 912和PA 1212中两种或三种的共聚酰胺;并且所述多羟基醇是季戊四醇、二季戊四醇和/或三季戊四醇;其中所述聚酰胺组合物如权利要求1至5中任一项所定义地构成。
12.根据权利要求11所述的方法,其中在所述聚酰胺组合物中至少一种聚酰胺和至少一种共聚酰胺的混合物的结晶点低于所述至少一种聚酰胺和至少一种共聚酰胺的结晶点。
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Also Published As
Publication number | Publication date |
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EP3714004A1 (de) | 2020-09-30 |
MX2020005347A (es) | 2020-08-13 |
EP3714004B1 (de) | 2023-10-04 |
CA3083050A1 (en) | 2019-05-31 |
JP7446996B2 (ja) | 2024-03-11 |
US20210198487A1 (en) | 2021-07-01 |
KR20200084047A (ko) | 2020-07-09 |
US11945949B2 (en) | 2024-04-02 |
WO2019101851A1 (de) | 2019-05-31 |
BR112020007184A2 (pt) | 2020-09-24 |
CN111344354A (zh) | 2020-06-26 |
JP2021504520A (ja) | 2021-02-15 |
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