CN1576317A - 基于聚醚酰胺的模制组合物 - Google Patents
基于聚醚酰胺的模制组合物 Download PDFInfo
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- CN1576317A CN1576317A CNA2004100712337A CN200410071233A CN1576317A CN 1576317 A CN1576317 A CN 1576317A CN A2004100712337 A CNA2004100712337 A CN A2004100712337A CN 200410071233 A CN200410071233 A CN 200410071233A CN 1576317 A CN1576317 A CN 1576317A
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- moulding compound
- weight
- polyetheramides
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- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims abstract description 10
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- 125000000524 functional group Chemical group 0.000 claims abstract description 3
- 125000001931 aliphatic group Chemical group 0.000 claims abstract 2
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- 238000000034 method Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 229920000570 polyether Polymers 0.000 claims description 5
- 229920001897 terpolymer Polymers 0.000 claims description 5
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- OFNISBHGPNMTMS-UHFFFAOYSA-N 3-methylideneoxolane-2,5-dione Chemical compound C=C1CC(=O)OC1=O OFNISBHGPNMTMS-UHFFFAOYSA-N 0.000 description 2
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- UTOVMEACOLCUCK-PLNGDYQASA-N butyl maleate Chemical compound CCCCOC(=O)\C=C/C(O)=O UTOVMEACOLCUCK-PLNGDYQASA-N 0.000 description 2
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- GTZCVFVGUGFEME-IWQZZHSRSA-N cis-aconitic acid Chemical compound OC(=O)C\C(C(O)=O)=C\C(O)=O GTZCVFVGUGFEME-IWQZZHSRSA-N 0.000 description 2
- 150000001990 dicarboxylic acid derivatives Chemical class 0.000 description 2
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- 239000001530 fumaric acid Substances 0.000 description 2
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- 230000003068 static effect Effects 0.000 description 2
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- PWGJDPKCLMLPJW-UHFFFAOYSA-N 1,8-diaminooctane Chemical compound NCCCCCCCCN PWGJDPKCLMLPJW-UHFFFAOYSA-N 0.000 description 1
- HECLRDQVFMWTQS-RGOKHQFPSA-N 1755-01-7 Chemical compound C1[C@H]2[C@@H]3CC=C[C@@H]3[C@@H]1C=C2 HECLRDQVFMWTQS-RGOKHQFPSA-N 0.000 description 1
- GOXQRTZXKQZDDN-UHFFFAOYSA-N 2-Ethylhexyl acrylate Chemical compound CCCCC(CC)COC(=O)C=C GOXQRTZXKQZDDN-UHFFFAOYSA-N 0.000 description 1
- WDQMWEYDKDCEHT-UHFFFAOYSA-N 2-ethylhexyl 2-methylprop-2-enoate Chemical compound CCCCC(CC)COC(=O)C(C)=C WDQMWEYDKDCEHT-UHFFFAOYSA-N 0.000 description 1
- CFVWNXQPGQOHRJ-UHFFFAOYSA-N 2-methylpropyl prop-2-enoate Chemical compound CC(C)COC(=O)C=C CFVWNXQPGQOHRJ-UHFFFAOYSA-N 0.000 description 1
- WTKWFNIIIXNTDO-UHFFFAOYSA-N 3-isocyanato-5-methyl-2-(trifluoromethyl)furan Chemical compound CC1=CC(N=C=O)=C(C(F)(F)F)O1 WTKWFNIIIXNTDO-UHFFFAOYSA-N 0.000 description 1
- CUXGDKOCSSIRKK-UHFFFAOYSA-N 7-methyloctyl prop-2-enoate Chemical compound CC(C)CCCCCCOC(=O)C=C CUXGDKOCSSIRKK-UHFFFAOYSA-N 0.000 description 1
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- 239000004953 Aliphatic polyamide Substances 0.000 description 1
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 description 1
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- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 description 1
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- 238000010168 coupling process Methods 0.000 description 1
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- 238000009826 distribution Methods 0.000 description 1
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- 230000000694 effects Effects 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- SUPCQIBBMFXVTL-UHFFFAOYSA-N ethyl 2-methylprop-2-enoate Chemical compound CCOC(=O)C(C)=C SUPCQIBBMFXVTL-UHFFFAOYSA-N 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000012760 heat stabilizer Substances 0.000 description 1
- LNMQRPPRQDGUDR-UHFFFAOYSA-N hexyl prop-2-enoate Chemical compound CCCCCCOC(=O)C=C LNMQRPPRQDGUDR-UHFFFAOYSA-N 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
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- 239000011630 iodine Substances 0.000 description 1
- PBOSTUDLECTMNL-UHFFFAOYSA-N lauryl acrylate Chemical compound CCCCCCCCCCCCOC(=O)C=C PBOSTUDLECTMNL-UHFFFAOYSA-N 0.000 description 1
- 230000003137 locomotive effect Effects 0.000 description 1
- 230000005923 long-lasting effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- ZQKXQUJXLSSJCH-UHFFFAOYSA-N melamine cyanurate Chemical compound NC1=NC(N)=NC(N)=N1.O=C1NC(=O)NC(=O)N1 ZQKXQUJXLSSJCH-UHFFFAOYSA-N 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- TVIDDXQYHWJXFK-UHFFFAOYSA-N n-Dodecanedioic acid Natural products OC(=O)CCCCCCCCCCC(O)=O TVIDDXQYHWJXFK-UHFFFAOYSA-N 0.000 description 1
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- RXOHFPCZGPKIRD-UHFFFAOYSA-N naphthalene-2,6-dicarboxylic acid Chemical compound C1=C(C(O)=O)C=CC2=CC(C(=O)O)=CC=C21 RXOHFPCZGPKIRD-UHFFFAOYSA-N 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- SXJVFQLYZSNZBT-UHFFFAOYSA-N nonane-1,9-diamine Chemical compound NCCCCCCCCCN SXJVFQLYZSNZBT-UHFFFAOYSA-N 0.000 description 1
- SJYNFBVQFBRSIB-UHFFFAOYSA-N norbornadiene Chemical compound C1=CC2C=CC1C2 SJYNFBVQFBRSIB-UHFFFAOYSA-N 0.000 description 1
- ANISOHQJBAQUQP-UHFFFAOYSA-N octyl prop-2-enoate Chemical class CCCCCCCCOC(=O)C=C ANISOHQJBAQUQP-UHFFFAOYSA-N 0.000 description 1
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical compound O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920006146 polyetheresteramide block copolymer Polymers 0.000 description 1
- 229920005996 polystyrene-poly(ethylene-butylene)-polystyrene Polymers 0.000 description 1
- 150000003141 primary amines Chemical group 0.000 description 1
- NHARPDSAXCBDDR-UHFFFAOYSA-N propyl 2-methylprop-2-enoate Chemical compound CCCOC(=O)C(C)=C NHARPDSAXCBDDR-UHFFFAOYSA-N 0.000 description 1
- PNXMTCDJUBJHQJ-UHFFFAOYSA-N propyl prop-2-enoate Chemical compound CCCOC(=O)C=C PNXMTCDJUBJHQJ-UHFFFAOYSA-N 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L79/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen or carbon only, not provided for in groups C08L61/00 - C08L77/00
-
- 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
-
- 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
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
- B29C48/09—Articles with cross-sections having partially or fully enclosed cavities, e.g. pipes or channels
-
- 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
- B29C49/00—Blow-moulding, i.e. blowing a preform or parison to a desired shape within a mould; Apparatus therefor
- B29C49/02—Combined blow-moulding and manufacture of the preform or the parison
- B29C49/04—Extrusion blow-moulding
-
- 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
-
- 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
- C08L77/12—Polyester-amides
-
- 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
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
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Abstract
模制组合物，包括下列成分：I.97－80重量份的聚醚酰胺，基于具有6－14个碳原子的线性脂肪族二胺、具有6－14个碳原子的线性脂肪族或芳香族二羧酸、和每个醚氧具有至少3个碳原子且在链端具有伯胺基团的聚醚二胺，II.3－20重量份的含有橡胶的官能团，其中I和II的总重量份为100。适用于柔性管的挤出，也适用于柔性吹塑成型制品的生产。
Description
技术领域
本发明涉及聚醚酰胺模制组合物，其具有优异的耐热成型性和抗水解性，且适合于软管的挤出和柔韧性吹塑制品的生产。
背景技术
增塑的部分结晶聚酰胺模制组合物，尤其是基于PA11或PA12的模制组合物，因为其优异的机械稳定性和耐化学性，很久以来就能通过挤出来将其生产成用于汽车制造的管件。然而，现在，在要求引擎盖下的使用温度越来越高的情况下，由于外增塑剂有挥发性，这些模制组合物在经过很短时间的使用后就会变硬。此外，在目前，当要求使用温度提高到110到150℃时，如果面对一定压力，它们会产生不可回复的变形趋势。尽管如EP-A-0095893所述，可以通过使用基于更高熔点的聚醚酯酰胺的模制组合物可以避免这些缺点，但是这一类型的聚酰胺弹性体不适于生产可用于上述使用目的的管材，因为满足了某使用目的下所需的耐水解性的相应的模制组合物，其远远达不到传统聚酰胺模制组合物的稳定性，且几周后就已失效了。
发明内容
因此本发明的任务在于生产具有高耐热成型性的抗水解模制组合物，该组合物具有高熔体粘度并从而可以很好地进行挤出和吹塑。所制得的模制品无须使用外增塑剂就应具有足够且能长期保持的柔软性以及很好的低温冲击强度。
通过包含有下列组分的模制组合物来实现这一目标：
I.97-80重量份，优选95-85重量份的聚醚酰胺，该聚醚酰胺基于具有6-14个碳原子的直链脂族二胺、具有6-14个碳原子的直链脂族或芳族二羧酸、和每个醚氧具有至少3个碳原子且在链端具有伯胺基团的聚醚二胺，
II.3-20重量份，优选5-15重量份，更优选为大于5-15重量份的含有官能基团的橡胶，
其中I和II的总重量份为100，
III.基于模制组合物的0-50重量％，优选0.1-30重量％，更优选1-20重量％的其它聚合物，以及
IV.基于模制组合物的0-10重量％的常规添加剂。
例如DE-OS3006961中就公开了基本的聚醚酰胺。然而，其中却并没有考虑将详细描述的基于己内酰胺或月桂内酰胺的聚醚酰胺用作组分I，因为一方面它们的熔点太低，另一方面它们的熔体粘度也太低。
本发明用来作为组分I的聚醚酰胺的熔点Tm(根据ISO 11357)优选为至少160℃，更优选为至少175℃；根据ISO 307，在23℃下并于0.5重量％的间甲酚溶液中测得的相对溶液粘度ηrel优选为至少1.80，更优选为1.85；并且根据ASTM D 4440，在220℃下并于机械频谱计(Kegel-Platte)中测得的静止剪切粘度优选为至少500Pas，更优选为至少800Pas。本发明所得的模制组合物，220℃时，同样根据ASTM D 4440的方法测量，应尽可能具有大于2000Pas的静止剪切粘度，优选大于5000Pas，因为如果不是这样就不可能稳定地并保持尺寸地挤出成型为理想的管材或其它成型件，或者只能在对于成本合算的成型生产来说是过于狭窄的一个温度范围内进行生产。
如果能得到或超过上述聚醚酰胺的溶体粘度或溶液粘度，那么组分II橡胶的加入就能毫无问题地导致理想的熔体粘度额外增加。
在制备聚醚酰胺时使用的二胺的实例是1，6-己二胺，1，8-辛二胺，1，9-壬二胺，1，10-癸二胺，1，12-十二甲撑二胺等。所使用的二羧酸的实例为己二酸，辛二酸，壬二酸，癸二酸，1，12-十二烷二酸，1，1 4-十四烷二酸，对苯二酸或2，6-萘二甲酸等。适宜的聚醚二胺是通过相应的聚醚二醇经还原性胺化作用进行转化，或通过丙烯腈偶合并其后进行氢化作用而得到的(例如，EP-A-0434244；EP-A-0296852)。它们通常都具有230-4000的数均分子量，在聚醚酰胺中的份数优选为5-50重量％。
由丙二醇得到的且商业可得的聚醚二胺是由Huntsman公司以JEFFAMIND型提供的。原则上，那些来自于1，4-丁二醇或1，3-丁二醇的聚醚二胺，或是混合构成的且具有得自二醇的单元的无规或嵌段分布的聚醚二胺也是十分合适的。所用的聚醚二酰胺的双官能度的理想值——用可乙酰化的氨基和羟基端基的摩尔份数表示——通常在至少95％，优选至少98％，如可由酸量滴定得出的二胺含量为至少90％，优选至少为95％。由于必须要得到高的摩尔质量，所以没有必要进一步要求所用的二羧酸与二胺和聚醚二胺总数更为相等。实际的氨基∶羧基的摩尔比率为0.98∶1至1.02∶1。
从要构造理想分子量的角度看，必须充分抑制那些能损坏端基或分解链段的副反应。因此，熔体缩聚反应的实际温度范围应限制在220℃-约245℃，其中的下限是由所基于的聚酰胺的熔点而得出的，上限是根据聚醚二胺开始热分解的温度而确定的。
令人吃惊的是，必须对最终要进行的固相后缩合作用选择剧烈的反应条件：经验表明，155-165℃的温度已足够满足脂族聚酰胺，如PA612，PA1010，PA1012或PA1212，而对于根据本发明所使用的、衍生自上述物质的聚醚酰胺却需要165-185℃的后缩合温度。为防止结块，固相后缩合温度应该在微晶熔点Tm以下不超过10K。对于技术人员来说，他们清楚地知道既可以在高真空状态下也可以在惰性气体流中进行后缩合作用。关于聚醚酰胺较低的后缩合活性的一个可能的原因是，它们的氨基端基由于一定程度上的空间位阻，其反应活性比一般的由脂族二胺得到的氨基端基要低。
所得到的聚醚酰胺中，优选至少30％的端基为氨基端基，更优选为至少50％的端基，特别优选至少60％的端基为氨基端基。
本发明所使用的橡胶是诸如选自下组中的共聚物：
-带有酸酐基团的乙烯-α-烯烃共聚物
-带有酸酐基团的苯乙烯-乙烯/丁烯嵌段共聚物
-乙烯-(甲基)丙烯酸缩水甘油酯共聚物
-乙烯-(甲基)丙烯酸酯-(甲基)丙烯酸缩水甘油酯三元共聚物，和/或
-乙烯-(甲基)丙烯酸酯-α，β-不饱和羧酸酐三元共聚物。
带有酸酐基团的乙烯-α-烯烃共聚物是使用公知的方法，通过将乙烯-α-烯烃共聚物和α，β-不饱和二羧酸酐或者它的前体，如马来酐、马来酸一丁酯、马来酸、反丁烯二酸、乌头酸、衣康酸或衣康酸酐通过自由基反应而制备。举例来说，乙烯-α-烯烃共聚物可以是乙烯含量为20-96重量％、优选为25-85重量％的乙烯/C3至C12-α-烯烃共聚物，或者可以是乙烯含量为20-96重量％、优选为25-85重量％的乙烯/C3至C12-α-烯烃/非共轭二烯的三元共聚物，其中具有至多约10重量％的非共轭二烯，例如双环[2.2.1]庚二烯，1，4-己二烯，双环戊二烯或5-亚乙基降冰片烯。举例来说，丙烯，1-丁烯，1-戊烯，1-己烯，1-辛烯，1-癸烯或1-十二碳烯适合作为C3至C12-α-烯烃。典型的例子是乙丙橡胶(EPM)，三元乙丙橡胶(EPDM)，乙烯-丁烯橡胶，LLDPE(线型低密度聚乙烯)以及VLDPE(极低密度聚乙烯)。这些共聚物通常含有0.5-6重量％、优选1-5重量％、更优选2-4重量％的衍生自α，β-不饱和二羧酸酐的单元。
所用的苯乙烯-乙烯/丁烯嵌段共聚物优选为苯乙烯-乙烯/丁烯-苯乙烯嵌段共聚物(SEBS)，它们是通过氢化苯乙烯-丁二烯-苯乙烯嵌段共聚物而得到的。然而，也可以使用二嵌段体系(SEB)或多嵌段体系。这类嵌段共聚物属于现有技术。含有酐基团的苯乙烯-乙烯/丁烯嵌段共聚物是通过已知的方法由苯乙烯-乙烯/丁烯嵌段共聚物和α，β-不饱和二羧酸酐或者其前体，例如马来酐、马来酸一丁酯、马来酸、反丁烯二酸、乌头酸、衣康酸或衣康酸酐之间的自由基反应得到的。这些嵌段共聚物通常含有0.5-6重量％、优选1-5重量％、更优选2-4重量％的从α，β-不饱和二羧酸酐衍生得到的单元。
实质上，乙烯-(甲基)丙烯酸缩水甘油酯共聚物通常含有的是以下单体的单元：
-20-98重量％，优选30-97重量％，更优选为40-96重量％的乙烯，和
-2-80重量％，优选3-70重量％，更优选为4-60重量％的丙烯酸缩水甘油酯和/或甲基丙烯酸缩水甘油酯。
实质上，乙烯-(甲基)丙烯酸酯-(甲基)丙烯酸缩水甘油酯三元共聚物通常含有的是以下单体的单元：
-20-97.9重量％，优选30-96.9重量％，更优选为40-95.9重量％的乙烯，
-0.1-78重量％，优选1-67重量％，更优选为2-56重量％的与C1至C12-醇生成的丙烯酸酯和/或甲基丙烯酸酯，和
-2-80重量％，优选3-70重量％，更优选为4-60重量％的丙烯酸缩水甘油酯和/或甲基丙烯酸缩水甘油酯，
其中，举例来说，所使用的丙烯酸酯或甲基丙烯酸酯是下列化合物：丙烯酸甲酯，丙烯酸乙酯，丙烯酸正丙酯，丙烯酸正丁酯，丙烯酸异丁酯，丙烯酸正己酯，丙烯酸正辛酯，丙烯酸-2-乙基己酯，丙烯酸异壬酯，丙烯酸十二酯，甲基丙烯酸甲酯，甲基丙烯酸乙酯，甲基丙烯酸正丙酯，甲基丙烯酸正丁酯，甲基丙烯酸异丁酯和/或甲基丙烯酸-2-乙基己酯。
实质上，乙烯-(甲基)丙烯酸酯-α，β-不饱和羧酸酐三元共聚物含有的是以下单体的单元：
-20-97.5重量％，优选30-95重量％，更优选为40-92重量％的乙烯，
-2-79.5重量％，优选4-69重量％，更优选为6-58重量％的丙烯酸酯或甲基丙烯酸酯，和
-0.5-6重量％，优选1-5重量％，更优选为2-4重量％的α，β-不饱和羧酸酐，
其中，可以将上述示例性提及的化合物作为丙烯酸酯或甲基丙烯酸酯以及作为α，β-不饱和羧酸酐或其前体来用。
适合的组分III的聚合物首先是那些与聚醚酰胺相容的物质，比如聚酰胺。优选选用其类型与聚醚酰胺的硬链段相同的聚酰胺。有利的是，聚酰胺具有至少为1.9的相对溶液粘度ηrel。
适宜的组分IV的添加剂首先是稳定剂，导电碳黑，阻燃剂如三聚氰胺氰尿酸酯，颜料和加工助剂。包括在组分III定义中的聚合物不在此列。
组分II的共聚物，以及适当情况下，组分III和IV的添加剂的加工，是在熔融的时候，并伴随着剪切，例如在双螺杆挤出机或共捏和机中进行。
本发明的模制组合物可以通过例如挤出，传统的吹塑或3D吹塑成型，例如通过开放半模中的软管挤出，3D软管操作或3D抽吸模塑，通过连续的吹塑成型为硬/软复合物，或通过其他吹塑成型方法来进行加工。
此外，模塑组合物还可以通过共挤出，共挤吹塑，共挤3D吹塑，共挤抽吸吹塑等，来形成多层复合物。
模制组合物也可以通过注塑法制备，也包括如GIT(气体内压技术)或WIT(水注入技术)等方法的变体。
根据所述的方法还可以制得诸如单层管或多层管。这些管子可以是光滑的也可以是部分或全部有褶皱的。模制组合物也可以用来生产任何形式的型材，如密封型材或中空体，例如容器。
本发明的模制品可例如用于机车制造，机械和设备的制造以及药物技术中，尤其是作为制动加力器的低压导管，空气管路，耐压胶管，如压缩空气管，控制管，冷却剂管，输油管，通风管，挡风玻璃清洗设备管，液压离合器系统的管线，侍服器控制管线，机动车辆空调设备的管线，电缆包皮层或电线包皮层，机械或设备制造领域内的或药物技术中的管线或作为滤油器或燃料过滤器的注射成模部件的管线。这些模制品同样都是本发明的内容之一。
通过下面的实施例阐述本发明。
具体实施方式
聚醚酰胺的制备：
200L的搅动式高压釜装有下列起始反应物料：
26.11kg 75％的1，6-己二胺水溶液，
52.94kg的1.12-十二烷二酸，
25.55kg的JEFFAMIND400以及
100g 50％的次磷酸水溶液。
起始物料在氮气氛下熔融并在密封的高压釜中加热搅拌至约220℃，同时将内压调节为约20bar。保持该压力2小时，之后溶体再加热到230℃，并且其间连续减压至大气压力，在氮气流中保持该温度1.5小时。接着在3小时内，容器抽空至28mbar，并在此压力下再保持3小时，直至扭矩表明，熔体的粘度不再上升。再用齿轮泵将熔体放出，并粒化成小条状。这些颗粒在80℃下于氮气中干燥24小时。
产品具有以下特征值：
微晶熔点Tm：193℃
相对溶液粘度ηrel：1.91
COOH端基：21mmol/kg
氨基端基：26mmol/kg
由所使用单体的比率得到在该聚醚酰胺中正式的PA612嵌段的平均摩尔质量为1083。
将50kg的这些颗粒在容量为250升的滚筒式干燥机中于175℃的套管温度下，并在氮气中(250l/h)中后浓缩24小时。经过这段时间后，产品具有以下特征值：
微晶熔点Tm：193℃
相对溶液粘度ηrel：2.06
COOH端基：14mmol/kg
氨基端基：20mmol/kg
模制组合物的制备：
以下给出以重量份计的模制组合物配方。将各个配方组分加入到Werner & Pfleiderer公司的双螺杆挤出机中，桶温为250℃。
表1：实施例
| 组分 | 对照 | 1 | 2 | 3 | 4 | 5 | 6 |
| 聚醚酰胺 | 97.25 | 94.25 | 92.25 | 87.25 | 82.25 | 92.25 | 82.25 |
| PA612，氨基端基过量；ηrel＝2.25 | - | - | - | 5.0 | 10.0 | - | 10.0 |
| EXXELORVA 1803(根据生产手册，EPM橡胶含有约0.7重量％的接枝的马来酸酐) | - | 3.0 | 5.0 | 5.0 | 5.0 | - | - |
| 乙烯-丙烯酸酯-甲基丙烯酸缩水甘油酯三元共聚物；重量份为：60/32/8 | - | - | - | - | - | 5.0 | 5.0 |
| 胺热稳定剂 | 0.50 | 0.50 | 0.50 | 0.50 | 0.50 | 0.50 | 0.50 |
| 碘基稳定剂配料 | 1.00 | 1.00 | 1.00 | 1.00 | 1.00 | 1.00 | 1.00 |
| 黑色着色剂颗粒 | 1.25 | 1.25 | 1.25 | 1.25 | 1.25 | 1.25 | 1.25 |
| Ceasit PC(硬脂酸钙；外部) | 0.04 | 0.04 | 0.04 | 0.04 | 0.04 | 0.04 | 0.04 |
| 根据ISO 179/leA的缺口冲击强度[kJ/m2] 23℃-40℃ | 413.1 | 814.9 | 1136.5 | 1187.5 | 1207.8 | 1094.9 | 1155.9 |
| 根据ISO 527的拉伸弹性模量[MPa] | 550 | 510 | 490 | 520 | 550 | 480 | 570 |
从中看出，如果通过同时添加聚酰胺来弥补由于橡胶的添加而引起的弹性模量的有限下降，则在室温下和在-40℃下均能获得明显改善的缺口冲击强度。弹性模量可以通过成分的混合比率而调节到所期望的值。
实施例1-6所得到的模制组合物的熔融粘度比对照的模制组合物要高，同时，它们具有更好的结构粘度(熔融粘度的升高取决于剪切力)，这就使得它们尤其适合于挤出成型或吹塑成型。
Claims (21)
1.模制组合物，其包含下列组分：
I.97-80重量份的聚醚酰胺，该聚醚酰胺基于具有6-14个碳原子的直链脂族二胺、具有6-14个碳原子的直链脂族或芳族二羧酸和每个醚氧具有至少3个碳原子且在链端具有伯胺基团的聚醚二胺，
II.3-20重量份的含有官能基团的橡胶，
其中I和II的总重量份为100。
2.权利要求1的模制组合物，其特征在于，
所含组分I的量为95-85重量份，所含组分II的量为5-15重量份。
3.上述权利要求之一的模制组合物，其特征在于，
所含组分II的量为大于5重量％。
4.上述权利要求之一的模制组合物，其特征在于，
组分I的聚醚酰胺的微晶熔点Tm为至少160℃。
5.权利要求4所述的模制组合物，其特征在于，
微晶熔点Tm为至少175℃。
6.上述权利要求之一的模制组合物，其特征在于，
聚醚酰胺的相对溶液粘度ηrel为至少1.80。
7.权利要求6的模制组合物，其特征在于，
聚醚酰胺的相对溶液粘度ηrel为至少1.85。
8.上述权利要求之一的模制组合物，其特征在于，
220℃时，聚醚酰胺的零剪切粘度为至少500Pas。
9.权利要求8的模制组合物，其特征在于，
220℃时，聚醚酰胺的零剪切粘度为至少800Pas。
10.上述权利要求之一的模制组合物，其特征在于，
用来制备聚醚酰胺的聚醚二胺的数均分子量为230-4000。
11.上述权利要求之一的模制组合物，其特征在于，
衍生自聚醚二胺的聚醚酰胺的分数为5-50重量％。
12.上述权利要求之一的模制组合物，其特征在于，
220℃时，其零剪切粘度为至少2000Pas。
13.权利要求12的模制组合物，其特征在于，
220℃时，其零剪切粘度为至少5000Pas。
14.上述权利要求之一的模制组合物，其特征在于，
以模制组合物计，它包含最多50重量％的其它聚合物。
15.上述权利要求之一的模制组合物，其特征在于，
以模制组合物计，它包含最多10重量％的常规添加剂。
16.上述权利要求之一的模制组合物，其特征在于，
组分II选自下组：
-含有酸酐基团的乙烯-α-烯烃共聚物，
-含有酸酐基团的苯乙烯-乙烯/丁烯嵌段共聚物，
-乙烯-(甲基)丙烯酸缩水甘油酯共聚物，
-乙烯-(甲基)丙烯酸酯-(甲基)丙烯酸缩水甘油酯三元共聚物，和/或
-乙烯-(甲基)丙烯酸酯-α，β-不饱和羧酸酐三元共聚物。
17.由上述权利要求之一的模制组合物制得的成型件。
18.权利要求17的成型件，通过挤出成型、共挤出成型、吹塑成型、3D吹塑成型、共挤出吹塑成型、共挤出3D吹塑成型、共挤出抽吸吹塑成型或注塑成型制得。
19.权利要求17或18的成型件，其特征在于，
它是单层管、多层管、型材或中空体。
20.权利要求17-19之一的成型件，其特征在于，
它是制动加力器的低压导管，导气管，压缩空气管，控制管，冷却剂管，燃料管，通风管，挡风玻璃清洗设备管，液压离合器系统的管线，侍服器控制管线，机动车空调设备的管线，电缆包皮层或电线包皮层，机械或设备制造领域或药物技术用管，或滤油器或燃料过滤器的注射成模部件。
21.权利要求1-16之一的模制组合物的用途，用于通过挤出或吹塑来生产成型件。
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| DE10333005A DE10333005A1 (de) | 2003-07-18 | 2003-07-18 | Formmasse auf Basis von Polyetheramiden |
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| DE10064338A1 (de) * | 2000-12-21 | 2002-06-27 | Degussa | Formmasse mit guter Blasformbarkeit |
| DE10161038A1 (de) * | 2001-12-12 | 2003-06-26 | Degussa | pH-Wert geregeltes Polyamidpulver für Kosmetikanwendungen |
| DE10164408A1 (de) * | 2001-12-28 | 2003-07-17 | Degussa | Flüssigkeits- oder dampfführendes System mit einer Fügezone aus einem coextrudierten Mehrschichtverbund |
| DE10201903A1 (de) * | 2002-01-19 | 2003-07-31 | Degussa | Formmasse auf Basis von Polyetheramiden |
| DE10228439A1 (de) * | 2002-06-26 | 2004-01-22 | Degussa Ag | Kunststoff-Lichtwellenleiter |
| ATE383939T1 (de) * | 2002-09-21 | 2008-02-15 | Evonik Degussa Gmbh | Verfahren zur herstellung eines dreidimensionalen objektes |
| DE10245355A1 (de) * | 2002-09-27 | 2004-04-08 | Degussa Ag | Rohrverbindung |
| US7160669B2 (en) * | 2002-10-16 | 2007-01-09 | Sumitomo Chemical Company, Limited | Chemical amplification type resist composition |
| DE10248406A1 (de) | 2002-10-17 | 2004-04-29 | Degussa Ag | Laser-Sinter-Pulver mit Titandioxidpartikeln, Verfahren zu dessen Herstellung und Formkörper, hergestellt aus diesem Laser-Sinterpulver |
| EP1413594A2 (de) * | 2002-10-17 | 2004-04-28 | Degussa AG | Laser-Sinter-Pulver mit verbesserten Recyclingeigenschaften, Verfahren zu dessen Herstellung und Verwendung des Laser-Sinter-Pulvers |
| DE10250330A1 (de) * | 2002-10-29 | 2004-05-13 | Degussa Ag | Biegeelement mit drehsinnabhängigem Verhalten |
| DE10251790A1 (de) * | 2002-11-07 | 2004-05-19 | Degussa Ag | Polyamidpulver mit dauerhafter, gleichbleibend guter Rieselfähigkeit |
| DE50302649D1 (de) * | 2002-11-28 | 2006-05-11 | Degussa | Laser-Sinter-Pulver mit Metallseifen, Verfahren zu dessen Herstellung und Formkörper, hergestellt aus diesem Laser-Sinter-Pulver |
| DE10311437A1 (de) * | 2003-03-15 | 2004-09-23 | Degussa Ag | Laser-Sinter-Pulver mit PMMI, PMMA und/oder PMMI-PMMA-Copolymeren, Verfahren zu dessen Herstellung und Formkörper, hergestellt aus diesem Laser-Sinterpulver |
| EP1459871B1 (de) | 2003-03-15 | 2011-04-06 | Evonik Degussa GmbH | Verfahren und Vorrichtung zur Herstellung von dreidimensionalen Objekten mittels Mikrowellenstrahlung sowie dadurch hergestellter Formkörper |
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| DE10334497A1 (de) * | 2003-07-29 | 2005-02-24 | Degussa Ag | Polymerpulver mit phosphonatbasierendem Flammschutzmittel, Verfahren zu dessen Herstellung und Formkörper, hergestellt aus diesem Polymerpulver |
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| DE10337707A1 (de) * | 2003-08-16 | 2005-04-07 | Degussa Ag | Verfahren zur Erhöhung des Molekulargewichts bei Polyamiden |
-
2003
- 2003-07-18 DE DE10333005A patent/DE10333005A1/de not_active Withdrawn
-
2004
- 2004-05-24 EP EP04102259.1A patent/EP1518901B1/de not_active Expired - Lifetime
- 2004-07-02 MX MXPA04006556A patent/MXPA04006556A/es active IP Right Grant
- 2004-07-15 JP JP2004209065A patent/JP5185490B2/ja not_active Expired - Lifetime
- 2004-07-15 BR BRPI0402747-7A patent/BRPI0402747B1/pt active IP Right Grant
- 2004-07-16 US US10/892,089 patent/US7582342B2/en active Active
- 2004-07-16 NO NO20043051A patent/NO20043051L/no unknown
- 2004-07-16 CN CNB2004100712337A patent/CN100422262C/zh not_active Expired - Lifetime
- 2004-07-16 KR KR1020040055483A patent/KR101062627B1/ko active IP Right Grant
- 2004-07-16 CA CA002474992A patent/CA2474992A1/en not_active Abandoned
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102227465B (zh) * | 2008-12-01 | 2016-11-09 | 赢创德固赛有限责任公司 | 生产具有提高的熔体劲度的模塑组合物或模塑制品的方法 |
| CN102227465A (zh) * | 2008-12-01 | 2011-10-26 | 赢创德固赛有限责任公司 | 生产具有提高的熔体劲度的模塑组合物或模塑制品的方法 |
| CN107428933A (zh) * | 2015-04-10 | 2017-12-01 | 株式会社普利司通 | 聚酰胺系热塑性弹性体和轮胎 |
| CN107428933B (zh) * | 2015-04-10 | 2020-07-03 | 株式会社普利司通 | 聚酰胺系热塑性弹性体和轮胎 |
| US10766304B2 (en) | 2015-04-10 | 2020-09-08 | Bridgestone Corporation | Polyamide-based thermoplastic elastomer and tire |
| CN112867755B (zh) * | 2018-10-16 | 2024-01-02 | 赢创运营有限公司 | 聚醚嵌段酰胺-聚(甲基)丙烯酸系物泡沫 |
| CN112867755A (zh) * | 2018-10-16 | 2021-05-28 | 罗姆化学有限责任公司 | 聚醚嵌段酰胺-聚(甲基)丙烯酸系物泡沫 |
| CN111334035A (zh) * | 2018-12-19 | 2020-06-26 | Ems 专利股份公司 | 用于挤出吹塑的聚酰胺模制组合物 |
| CN111334035B (zh) * | 2018-12-19 | 2023-12-19 | Ems 专利股份公司 | 用于挤出吹塑的聚酰胺模制组合物 |
| CN114981337A (zh) * | 2019-12-19 | 2022-08-30 | 赢创运营有限公司 | 包含聚醚嵌段酰胺的模塑组合物 |
| CN114981337B (zh) * | 2019-12-19 | 2023-07-14 | 赢创运营有限公司 | 包含聚醚嵌段酰胺的模塑组合物 |
| WO2021120091A1 (en) * | 2019-12-19 | 2021-06-24 | Evonik Operations Gmbh | Moulding composition comprising polyether block amide |
| CN114654658A (zh) * | 2022-03-17 | 2022-06-24 | 杭州恒新塑业有限公司 | 一体式高分子包装容器成型设备 |
Also Published As
| Publication number | Publication date |
|---|---|
| NO20043051L (no) | 2005-01-19 |
| EP1518901B1 (de) | 2016-05-18 |
| EP1518901A2 (de) | 2005-03-30 |
| US7582342B2 (en) | 2009-09-01 |
| BRPI0402747A (pt) | 2005-05-24 |
| EP1518901A3 (de) | 2005-12-28 |
| JP5185490B2 (ja) | 2013-04-17 |
| KR101062627B1 (ko) | 2011-09-07 |
| BRPI0402747B1 (pt) | 2020-11-03 |
| CN100422262C (zh) | 2008-10-01 |
| MXPA04006556A (es) | 2005-03-31 |
| CA2474992A1 (en) | 2005-01-18 |
| KR20050009228A (ko) | 2005-01-24 |
| DE10333005A1 (de) | 2005-02-03 |
| JP2005042111A (ja) | 2005-02-17 |
| US20050014842A1 (en) | 2005-01-20 |
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