CN107922711A - 制造热成形制品的聚合物组合物 - Google Patents
制造热成形制品的聚合物组合物 Download PDFInfo
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- CN107922711A CN107922711A CN201680044889.0A CN201680044889A CN107922711A CN 107922711 A CN107922711 A CN 107922711A CN 201680044889 A CN201680044889 A CN 201680044889A CN 107922711 A CN107922711 A CN 107922711A
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- Prior art keywords
- poly
- acid
- carbodiimide
- ester
- polymer composition
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- 239000000203 mixture Substances 0.000 title claims abstract description 92
- 229920000642 polymer Polymers 0.000 title claims abstract description 28
- 238000004519 manufacturing process Methods 0.000 title description 10
- -1 saturated aliphatic dicarboxylic acids Chemical class 0.000 claims abstract description 99
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 61
- 229920000728 polyester Polymers 0.000 claims abstract description 53
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims abstract description 42
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 150000002009 diols Chemical class 0.000 claims abstract description 28
- 125000001931 aliphatic group Chemical group 0.000 claims abstract description 27
- 150000001875 compounds Chemical class 0.000 claims abstract description 25
- 125000000524 functional group Chemical group 0.000 claims abstract description 15
- 125000003118 aryl group Chemical group 0.000 claims abstract description 13
- 230000007062 hydrolysis Effects 0.000 claims abstract description 10
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 10
- 239000000945 filler Substances 0.000 claims abstract description 9
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- 239000005014 poly(hydroxyalkanoate) Substances 0.000 claims abstract description 6
- 229920000903 polyhydroxyalkanoate Polymers 0.000 claims abstract description 6
- VPKDCDLSJZCGKE-UHFFFAOYSA-N carbodiimide group Chemical group N=C=N VPKDCDLSJZCGKE-UHFFFAOYSA-N 0.000 claims abstract description 4
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- 238000010348 incorporation Methods 0.000 claims description 14
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 10
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- FEKRFYZGYUTGRY-UHFFFAOYSA-N n'-ethylmethanediimine Chemical compound CCN=C=N FEKRFYZGYUTGRY-UHFFFAOYSA-N 0.000 claims description 6
- 235000013361 beverage Nutrition 0.000 claims description 5
- 229960005137 succinic acid Drugs 0.000 claims description 4
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- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims description 3
- OBNCKNCVKJNDBV-UHFFFAOYSA-N ethyl butyrate Chemical compound CCCC(=O)OCC OBNCKNCVKJNDBV-UHFFFAOYSA-N 0.000 claims description 3
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 3
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- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 claims description 2
- 229940006015 4-hydroxybutyric acid Drugs 0.000 claims description 2
- WKFYXTPAHITPNK-UHFFFAOYSA-N N=C=N.C(C)(C)C1=CC=CC=C1 Chemical compound N=C=N.C(C)(C)C1=CC=CC=C1 WKFYXTPAHITPNK-UHFFFAOYSA-N 0.000 claims description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N Propionic acid Chemical compound CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 2
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- 125000000843 phenylene group Chemical group C1(=C(C=CC=C1)*)* 0.000 claims description 2
- 229920000070 poly-3-hydroxybutyrate Polymers 0.000 claims description 2
- 229940070710 valerate Drugs 0.000 claims description 2
- FERIUCNNQQJTOY-UHFFFAOYSA-M Butyrate Chemical compound CCCC([O-])=O FERIUCNNQQJTOY-UHFFFAOYSA-M 0.000 claims 1
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- GXGJIOMUZAGVEH-UHFFFAOYSA-N Chamazulene Chemical group CCC1=CC=C(C)C2=CC=C(C)C2=C1 GXGJIOMUZAGVEH-UHFFFAOYSA-N 0.000 claims 1
- OHZYJJCFLBKLDN-UHFFFAOYSA-N N=C=N.C1(=CC=CC=C1)C Chemical compound N=C=N.C1(=CC=CC=C1)C OHZYJJCFLBKLDN-UHFFFAOYSA-N 0.000 claims 1
- 150000001412 amines Chemical class 0.000 claims 1
- 210000000481 breast Anatomy 0.000 claims 1
- XATSGKXHVKZFKL-UHFFFAOYSA-N cyclohexylmethylcyclohexane;methanediimine Chemical compound N=C=N.C1CCCCC1CC1CCCCC1 XATSGKXHVKZFKL-UHFFFAOYSA-N 0.000 claims 1
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 claims 1
- FRVOOSTVCDXSRG-UHFFFAOYSA-N methanediimine;3,5,5-trimethylcyclohex-2-en-1-one Chemical compound N=C=N.CC1=CC(=O)CC(C)(C)C1 FRVOOSTVCDXSRG-UHFFFAOYSA-N 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 11
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- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 63
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 35
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- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 18
- 235000011187 glycerol Nutrition 0.000 description 12
- 239000000463 material Substances 0.000 description 12
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 239000004310 lactic acid Substances 0.000 description 9
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- 150000005846 sugar alcohols Polymers 0.000 description 9
- 239000004014 plasticizer Substances 0.000 description 8
- 150000003839 salts Chemical class 0.000 description 8
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 239000012948 isocyanate Substances 0.000 description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- CHTHALBTIRVDBM-UHFFFAOYSA-N furan-2,5-dicarboxylic acid Chemical class OC(=O)C1=CC=C(C(O)=O)O1 CHTHALBTIRVDBM-UHFFFAOYSA-N 0.000 description 6
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 6
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 description 6
- 239000004970 Chain extender Substances 0.000 description 5
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000003431 cross linking reagent Substances 0.000 description 5
- 229920001223 polyethylene glycol Polymers 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 229920000305 Nylon 6,10 Polymers 0.000 description 4
- 239000004952 Polyamide Substances 0.000 description 4
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- 229910000831 Steel Inorganic materials 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Natural products CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 4
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- 239000010959 steel Substances 0.000 description 4
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 3
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Abstract
本发明涉及尤其适合于在制造热成形制品中使用的聚合物组合物，它在工业堆肥中可生物降解。本发明还涉及生产所述组合物的方法和由此获得的制品。该聚合物组合物包括，相对于组分i.‑iv.之和，i)20‑60wt％至少一种聚酯，所述聚酯包括：a)二羧酸组分，所述二羧酸组分相对于全部二羧酸组分包含：a1)0‑20mol％由至少一种芳族二羧酸衍生的单元，a2)80‑100mol％由至少一种饱和脂族二羧酸衍生的单元，a3)0‑5mol％由至少一种不饱和脂族二羧酸衍生的单元；b)二醇组分，所述二醇组分相对于全部二醇组分包含：b1)95‑100mol％由至少一种饱和脂族二醇衍生的单元；b2)0‑5mol％由至少一种不饱和脂族二醇衍生的单元；ii)5‑35wt％至少一种聚羟基烷酸酯；iii)0.01‑5wt％的至少一种水解稳定剂，所述水解稳定剂包含具有二‑和/或多个官能团的至少一种化合物，该官能团包括碳二亚胺基团；iv)5‑50wt％至少一种填充剂。
Description
本发明涉及尤其适合于通过热成形来模塑的制品的制造中使用的聚合物组合物，它在工业堆肥中可生物降解。
本发明还涉及所述组合物的生产方法和由此获得的制品。
正如已知的，热模塑塑料材料的技术，例如热成形主要应用于生产具有高抗变形性的制品，例如容器，浴盆，板或分配饮料的小容器(capsule)，其中壁的厚度典型地大于200微米。
尽管制造具有这种大厚度的制品会确保所需的抗变形性能，但当这些制品用本身可生物降解的聚合物制造时，确保这些制品具有可崩解性能，从而使得它们适用于工业堆肥用装置产生难度。
鉴于上述问题，期望具有能经济且量产地转变成热成形制品且没有负面影响可堆肥性的组合物。
现已令人惊奇地发现，借助包括下述的用于生产热成形制品的聚合物组合物，可满足这一要求：
i)相对于组分i.-iv.之和，20-60wt％，优选30-50wt％至少一种聚酯，所述聚酯包括：
a)相对于全部二羧酸组分，含下述的二羧酸组分：
a1)0-20mol％，优选0-10mol％由至少一种芳族二羧酸衍生的单元，
a2)80-100mol％，优选90-100mol％由至少一种饱和脂族二羧酸衍生的单元，
a3)0-5mol％，优选0.1-1mol％，更优选0.2-0.7mol％由至少一种不饱和脂族二羧酸衍生的单元；
b)相对于全部二醇组分，含下述的二醇组分：
b1)95-100mol％，优选97-100mol％由至少一种饱和脂族二醇衍生的单元；
b2)0-5mol％，优选0-3mol％由至少一种不饱和脂族二醇衍生的单元；
ii)相对于组分i.-iv.之和，5-35wt％，优选10-20wt％至少一种聚羟基烷酸酯；
iii)相对于组分i.-iv.之和，0.01-5wt％，优选0.02-3wt％至少一种水解稳定剂，所述水解稳定剂包含具有二-和/或多个官能团的至少一种化合物，该官能团包括碳二亚胺基团；
iv)相对于组分i.-iv.之和，5-50wt％，优选10-40wt％至少一种填充剂。
关于根据本发明组合物的聚酯，这些包括二羧酸组分，所述二羧酸组分包括相对于全部二羧酸组分，0-20mol％，优选0-10mol％由至少一种芳族二羧酸衍生的单元和80-100mol％，优选90-100mol％由至少一种饱和脂族二羧酸衍生的单元，和0-5mol％，优选0.1-1mol％，更优选0.2-0.7mol％由至少一种不饱和脂族二羧酸衍生的单元。
芳族二羧酸优选选自苯二甲酸类型的芳族二羧酸，优选对苯二甲酸或间苯二甲酸，更优选对苯二甲酸，和杂环二羧酸，优选2,5-呋喃二羧酸，2,4-呋喃二羧酸，2,3-呋喃二羧酸，3,4-呋喃二羧酸，更优选2,5-呋喃二羧酸，它们的酯，它们的盐和它们的混合物。在优选的实施方案中，所述芳族二羧酸包括：
-从1至99mol％，优选5至95％和更优选10至80％对苯二甲酸，它的酯或其盐；
-从99至1mol％，优选95至5％和更优选90至20％的2,5-呋喃二羧酸，它的酯或其盐。
饱和脂族二羧酸优选选自C2-C24，优选C4-C13，更优选C4-C11饱和二羧酸，它们的C1-C24，优选C1-C4烷基酯，它们的盐及其混合物。
优选的饱和脂族二羧酸选自琥珀酸，2-乙基琥珀酸，戊二酸，2-甲基戊二酸，己二酸，庚二酸，辛二酸，壬二酸，癸二酸，十一烷二酸，十二烷二酸，十三烷二酸和它们的C1-24烷基酯。
在本发明的优选实施方案中，饱和脂族二羧酸包括混合物，该混合物包含至少50mol％，优选大于60mol％，更优选大于65mol％琥珀酸，己二酸，壬二酸，癸二酸，十三烷二酸，它们的C1-C24，优选C1-C4酯及其混合物。
不饱和脂族二羧酸优选选自衣康酸，富马酸，4-亚甲基-庚二酸，3,4-双(亚甲基)壬二酸，5-亚甲基-壬二酸，它们的C1-C24，优选C1-C4烷基酯，它们的盐及其混合物。
在本发明的优选实施方案中，不饱和脂族二羧酸包括混合物，该混合物包含至少50mol％，优选大于60mol％，更优选大于65mol％衣康酸，它的C1-C24，优选C1-C4酯。更优选不饱和脂族二羧酸包括衣康酸。
根据本发明组合物的聚酯中的二醇组分包括95-100mol％，优选97-100mol％由至少一种饱和脂族二醇衍生的单元，相对于全部二醇组分，和0-5mol％，优选0-3mol％由至少一种不饱和脂族二醇衍生的单元，相对于全部二醇组分。
在优选的实施方案中，根据本发明组合物的聚酯中的二醇组分由饱和脂族二醇组成。
关于饱和脂族二醇，这些优选选自1,2-乙二醇，1,2-丙二醇，1,3-丙二醇，1,4-丁二醇，1,5-戊二醇，1,6-己二醇，1,7-庚二醇，1,8-辛二醇，1,9-壬二醇，1,10-癸二醇，1,11-十一烷二醇，1,12-十二烷二醇，1,13-十三烷二醇，1,4-环己烷二甲醇，新戊二醇，2-甲基-1,3-丙二醇，二脱水山梨醇，二脱水甘露醇，二脱水艾杜糖醇，环己二醇，环己烷甲二醇，二亚烷基二醇和分子量为100-4000的聚亚烷基二醇，例如聚乙二醇，聚丙二醇及其混合物。优选二醇组分包括至少50mol％选自1,2-乙二醇，1,3-丙二醇，1,4-丁二醇中的一种或多种二醇。更优选二醇组分包括1,4-丁二醇，或由1,4-丁二醇组成。
关于不饱和脂族二醇，这些优选选自顺式2-丁烯-1,4-二醇，反式2-丁烯-1,4-二醇，2-丁炔-1,4-二醇，顺式2-戊烯-1,5-二醇，反式2-戊烯-1,5-二醇，2-戊炔-1,5-二醇，顺式2-己烯-1,6-二醇，反式2-己烯-1,6-二醇，2-己炔-1,6-二醇，顺式3-己烯-1,6-二醇，反式3-己烯-1,6-二醇，3-己炔-1,6-二醇。
关于组合物中的聚酯i,，这些优选选自脂族聚酯("AP")和脂族-芳族聚酯("AAPE")。
在本发明的意义上，脂族聚酯AP是指含二羧酸组分和二醇组分的聚酯，所述二羧酸组分由相对于二羧酸组分的总摩尔数，95-100mol％至少一种饱和脂族二羧酸和0-5mol％至少一种不饱和脂族二羧酸组成，所述二醇组分包括相对于二醇组分的总摩尔数，95-100mol％由至少一种饱和脂族二醇衍生的单元和0-5mol％由至少一种不饱和脂族二醇衍生的单元。
在本发明中，AAPE聚酯是指含二羧酸组分和二醇组分的聚酯，所述二羧酸组分由至少一种芳族二羧酸化合物，至少一种饱和脂族二羧酸，和相对于二羧酸组分的总摩尔数，0-5mol％至少一种不饱和脂族二羧酸组成，所述二醇组分包括相对于二醇组分的总摩尔数，95-100mol％由至少一种饱和脂族二醇衍生的单元和0-5mol％由至少一种不饱和脂族二醇衍生的单元。
在AP脂族聚酯情况下，优选的那些是聚酯，其中二羧酸组分包括由至少一种C2-C24，优选C4-C13，更优选C4-C11饱和脂族二羧酸，它们的C1-C24，优选C1-C4烷基酯，它们的盐及其混合物衍生的单元，和二醇组分包括由至少一种饱和脂族二醇的单元，其优选选自1,2-乙二醇，1,2-丙二醇，1,3-丙二醇，1,4-丁二醇。
在本发明的优选实施方案中，组合物中的聚酯i.包括至少一种脂族聚酯(AP)，优选聚(琥珀酸1,4-丁二醇酯)，聚(己二酸1,4-丁二醇酯)，聚(壬二酸1,4-丁二醇酯)，聚(癸二酸1,4-丁二醇酯)，聚(己二酸1,4-丁二醇酯-共-琥珀酸1,4-丁二醇酯)，聚(壬二酸1,4-丁二醇酯-共-琥珀酸1,4-丁二醇酯)，聚(癸二酸1,4-丁二醇酯-共-琥珀酸1,4-丁二醇酯)，聚(琥珀酸1,4-丁二醇酯-共-己二酸1,4-丁二醇酯-共-壬二酸1,4-丁二醇酯)。在特别优选的实施方案中，所述脂族聚酯是聚(琥珀酸1,4-丁二醇酯)。
在本发明的进一步优选的实施方案中，组合物中的聚酯包括至少一种脂族-芳族聚酯(AAPE)，并且有利地选自：
(A)包含由苯二甲酸类型的芳族二羧酸，优选对苯二甲酸，脂族二羧酸和脂族二醇衍生的重复单元的聚酯(AAPE-A)，其特征在于芳族单元含量为35至60mol％，优选40至55mol％，相对于二羧酸组分的总摩尔数。AAPE-A聚酯优选选自：聚(己二酸1,4-丁二醇酯-共-对苯二甲酸1,4-丁二醇酯)，聚(癸二酸1,4-丁二醇酯-共-对苯二甲酸1,4-丁二醇酯)，聚(壬二酸1,4-丁二醇酯-共-对苯二甲酸1,4-丁二醇酯)，聚(十三烷二酸1,4-丁二醇酯-共-对苯二甲酸1,4-丁二醇酯)，聚(琥珀酸1,4-丁二醇酯-共-对苯二甲酸1,4-丁二醇酯)，聚(己二酸1,4-丁二醇酯-共-癸二酸1,4-丁二醇酯-共-对苯二甲酸1,4-丁二醇酯)，聚(壬二酸1,4-丁二醇酯-共-癸二酸1,4-丁二醇酯-共-对苯二甲酸1,4-丁二醇酯)，聚(己二酸1,4-丁二醇酯-共-壬二酸1,4-丁二醇酯-共-对苯二甲酸1,4-丁二醇酯)，聚(琥珀酸1,4-丁二醇酯-共-癸二酸1,4-丁二醇酯-共-对苯二甲酸1,4-丁二醇酯)，聚(己二酸1,4-丁二醇酯-共-琥珀酸1,4-丁二醇酯-共-对苯二甲酸1,4-丁二醇酯)，聚(壬二酸1,4-丁二醇酯-共-琥珀酸1,4-丁二醇酯-共-对苯二甲酸1,4-丁二醇酯)。
(B)包含由杂环二羧酸，优选2,5-呋喃二羧酸，脂族二羧酸和脂族二醇衍生的重复单元的聚酯(AAPE-B)，其特征在于芳族单元含量为50至80mol％，优选60至75mol％，相对于二羧酸组分的总摩尔数。AAPE-B聚酯优选选自：聚(己二酸1,4-丁二醇酯-共-2,5-呋喃二羧酸1,4-丁二醇酯)，聚(癸二酸1,4-丁二醇酯-共-2,5-呋喃二羧酸1,4-丁二醇酯)，聚(壬二酸1,4-丁二醇酯-共-2,5-呋喃二羧酸1,4-丁二醇酯)，聚(十三烷二酸1,4-丁二醇酯-共-2,5-呋喃二羧酸1,4-丁二醇酯)，聚(琥珀酸1,4-丁二醇酯-共-2,5-呋喃二羧酸1,4-丁二醇酯)，聚(己二酸1,4-丁二醇酯-共-癸二酸1,4-丁二醇酯-共-2,5-呋喃二羧酸1,4-丁二醇酯)，聚(壬二酸1,4-丁二醇酯-共-癸二酸1,4-丁二醇酯-共-2,5-呋喃二羧酸1,4-丁二醇酯)，聚(己二酸1,4-丁二醇酯-共-壬二酸1,4-丁二醇酯-共-2,5-呋喃二羧酸1,4-丁二醇酯)，聚(琥珀酸1,4-丁二醇酯-共-癸二酸1,4-丁二醇酯-共-2,5-呋喃二羧酸1,4-丁二醇酯)，聚(己二酸1,4-丁二醇酯-共-琥珀酸1,4-丁二醇酯-共-2,5-呋喃二羧酸1,4-丁二醇酯)，聚(壬二酸1,4-丁二醇酯-共-琥珀酸1,4-丁二醇酯-共-2,5-呋喃二羧酸1,4-丁二醇酯)。
除了二羧酸组分和二醇组分以外，根据本发明组合物的聚酯优选包括由相对于二羧酸组分的总摩尔数，用量为0至49％，优选0至30mol％的至少一种羟基酸衍生的重复单元。适当的羟基酸的实例是羟基乙酸，羟基丁酸，羟基己酸，羟基戊酸，7-羟基庚酸，8-羟基己酸，9-羟基壬酸，和乳酸或丙交酯。羟基酸可以原样插入到链内或者也可首先引起与二酸或二醇反应。
相对于二羧酸组分的总摩尔数，也可存在用量不大于10mol％长分子，所述长分子具有两个官能团，该官能团包含不在端基位置的官能团。实例是二聚体酸，蓖麻油酸和掺入环氧官能团的酸，以及分子量为200至10000的聚氧亚乙基。
相对于二羧酸组分的总摩尔数，也可存在百分比为最多30mol％的二胺，氨基酸，和氨基醇。
在本发明组合物中聚酯的制备期间，也可以有利地添加相对于二羧酸组分(以及任何羟基酸)的总摩尔数，用量为0.1至3mol％具有多个官能团的一个或多个分子以便获得支化产物。这些分子的实例是甘油，季戊四醇，三羟甲基丙烷，柠檬酸，二季戊四醇，酸甘油三酯，聚甘油。
本发明组合物中聚酯的分子量Mn优选为≥20000，更优选≥40000。关于分子量的多分散性指数Mw/Mn，它优选为1.5至10，更优选1.6至5，和甚至更优选1.8至2.7。
可借助凝胶渗透色谱法(GPC)测量分子量Mn和Mw。可采用维持在40℃下的色谱体系，使用一组串联的三个柱子(粒径5μm和孔隙度分别和折射指数检测仪，氯仿作为洗脱剂(流量1ml/min)并使用聚苯乙烯作为参考标准物进行测定。
根据本发明组合物中聚酯的末端酸基团含量优选为30至160meq/kg。
可按照下述方式测量末端酸基团含量：将1.5-3g聚酯与60ml氯仿一起置于100ml烧瓶内。在聚酯完全溶解之后添加25ml的2-丙醇，和立即在分析之前还添加1ml去离子水。相对于前面的标准化NaOH乙醇溶液滴定所得到的溶液。使用合适的指示剂，例如在非水性溶剂中用于酸-碱滴定的玻璃电极，测定滴定的终点。基于使用下述方程式消耗的NaOH乙醇溶液，计算末端酸基团含量：
其中：Veq＝在样品的滴定终点处，NaOH的乙醇溶液的ml；
Vb＝在空白滴定期间为实现pH＝9,5所要求的NaOH的乙醇溶液的ml；
T＝以摩尔/升表达的NaOH的乙醇溶液的浓度；
P＝以克计的样品重量。
优选地，根据本发明组合物的聚酯的特性粘度(针对在25℃下，浓度为0.2g/dl的CHCl3溶液，采用乌氏粘度计测量)大于0.3dl/g，优选为0.3至2dl/g，更优选0.4至1.3dl/g。
优选地，根据本发明组合物的聚酯是可生物降解的。在本发明的意义上，可生物降解的聚合物是指根据标准EN 13432可生物降解的聚合物。
可借助本领域已知的任何方法，合成根据本发明组合物的聚酯。特别地，它们可有利地通过缩聚反应获得。
有利地，可在合适的催化剂存在下进行该合成方法。在这种合适的催化剂当中，作为实例，可提及锡的有机金属化合物，例如锡酸的衍生物，钛化合物，例如钛酸正丁酯，铝化合物，例如三异丙基铝，锑和锌与锆的化合物，及其混合物。
为了确保热成形制品高的抗变形性能，本发明的组合物包括相对于组分i.-iv.之和，5-35wt％，优选10-20wt％至少一种聚羟基烷酸酯(组分ii.)，其优选选自乳酸的聚酯，聚-ε-己内酯，聚羟基丁酸酯，聚羟基丁酸酯戊酸酯，聚羟基丁酸酯丙酸酯，聚羟基丁酸酯-己酸酯，聚羟基丁酸酯-癸酸酯，聚羟基丁酸酯-十二烷酸酯，聚羟基丁酸酯-十六烷酸酯(esadecanoate)，聚羟基丁酸酯-十八烷酸酯，聚3-羟基丁酸酯-4-羟基丁酸酯。
优选地，组合物中的聚羟基烷酸酯包括至少80wt％乳酸的一种或多种聚酯。
在优选的实施方案中，乳酸的聚酯选自聚L乳酸，聚D乳酸，聚D-L乳酸立体复合物，含大于50mol％所述乳酸的聚酯的共聚物或它们的混合物。
尤其优选是分子量Mw大于50,000且剪切粘度为50至500Pa.s，优选100至300Pa.s(根据标准ASTM D3835，在T＝190℃，剪切速率＝1000s-1，D＝1mm，L/D＝10下测量)的含有至少95wt％由L-乳酸或D-乳酸或其组合衍生的重复单元的乳酸的聚酯。
在本发明尤其优选的实施方案中，乳酸的聚酯包括熔点范围为135-170℃，玻璃化转变温度(Tg)范围为55-65℃且MFR(根据标准ASTM-D1238，在190℃和2.16kg下测量)范围为1-50g/10min的至少95wt％由L-乳酸衍生的单元，≤5％由D-乳酸衍生的重复单元。具有前述性能的乳酸的聚酯的商业实例例如是IngeoTM商品名的产品Biopolymer 4043D，3251D和6202D。
根据本发明的组合物包括0.01-5wt％，优选0.02-3wt％，更优选0.1-1wt％至少一种水解稳定剂(组分iii.)，其改进对水解的稳定性且选自具有二-和/或多个官能团的化合物，该官能团引入碳二亚胺。
在本发明组合物中使用的具有掺入碳二亚胺基的二-和多个官能团的化合物优选选自聚(亚环辛基碳二亚胺)，聚(1,4-二亚甲基亚环己基碳二亚胺)，聚(二环己基甲烷碳二亚胺)，聚(亚环己基碳二亚胺)，聚(亚乙基碳二亚胺)，聚(亚丁基碳二亚胺)，聚(亚异丁基碳二亚胺)，聚(亚壬基碳二亚胺)，聚(亚十二烷基碳二亚胺)，聚(亚新戊基碳二亚胺)，聚(1,4-二亚甲基亚苯基碳二亚胺)，聚(2,2′,6,6′-四异丙基二亚苯基碳二亚胺)D)，聚(2,4,6-三异丙基-1,3-亚苯基碳二亚胺)P-100)，聚(2,6二异丙基-1,3-亚苯基碳二亚胺)P)，聚(甲苯基碳二亚胺)，聚(4,4′-二苯基甲烷碳二亚胺)，聚(3,3′-二甲基-4,4′-亚联苯基碳二亚胺)，聚(对亚苯基碳二亚胺)，聚(间亚苯基碳二亚胺)，聚(3,3'-二甲基-4,4′-二苯基甲烷碳二亚胺)，聚(亚萘基碳二亚胺)，聚(异佛尔酮碳二亚胺)，聚(枯烯碳二亚胺)，对亚苯基双(乙基碳二亚胺)，1,6-六亚甲基双(乙基碳二亚胺)，1,8-八亚甲基双(乙基碳二亚胺)，1,10-十亚甲基双(乙基碳二亚胺)，1,12-十二亚甲基双(乙基碳二亚胺)及其混合物。
本发明的组合物包括5-50wt％，优选10-40wt％的至少一种填充剂(组分iv.)，其有助于改进本发明热成形物品的耐变形性和尺寸稳定性且优选选自高岭土，重晶石，粘土，滑石，钙和镁的碳酸盐，铁和铅，氢氧化铝，硅藻土，硫酸铝，硫酸钡，二氧化硅，云母，二氧化钛，硅灰石，淀粉，甲壳素，壳聚糖，藻酸盐，蛋白质，例如明胶，玉米蛋白，干酪素，胶原蛋白，白明胶，天然橡胶，松香酸及其衍生物。
术语淀粉是指所有类型淀粉，也就是说，面粉，天然淀粉，水解淀粉，变性淀粉，糊化淀粉，塑化淀粉，热塑性淀粉，含复合淀粉的生物填料或其混合物。根据本发明尤其合适的是诸如土豆，玉米，木薯和豌豆淀粉之类的淀粉。
能够容易变性且具有较高起始分子量的淀粉，例如土豆淀粉和玉米淀粉被证明是尤其有利的。
淀粉可以原样存在或者以化学改性形式存在，例如取代度为0.2至2.5的淀粉酯形式，淀粉羟基丙酸酯，或用脂肪链改性的淀粉。
此处提到变性淀粉是指在专利EP-0 118 240和EP-0 327 505中包括的教导，这理解为是指按照下述方式处理的淀粉，所述方式使得它在光学显微镜下在偏振光中不具有所谓的"偏光十字(Maltese crosses)"和在相差显微镜下不具有所谓的"重影(ghos ts)"。
有利地，借助挤出工艺，在110至250℃，优选130至180℃的温度下，优选在0.1至7MPa，优选0.3-6MPa的压力下，使淀粉变性，从而优选在该挤出期间提供大于0.1kWh/kg的比能。
优选相对于淀粉的重量，在1-40wt％选自水和具有2至22个碳原子的多元醇中的一种或多种增塑剂存在下发生淀粉的变性。关于水，它可以是包括在淀粉中自然存在的水。在多元醇当中，优选是具有1至20个羟基含有2至6个碳原子的多元醇，它们的醚，硫醚，以及有机和无机酯。多元醇的实例是甘油，二甘油，聚甘油，季戊四醇，聚甘油乙氧基化物，乙二醇，聚乙二醇，1,2-丙二醇，1,3-丙二醇，1,4-丁二醇，新戊二醇，山梨醇单乙酸酯，山梨醇二乙酸酯，山梨醇单乙氧基化物，山梨醇二乙氧基化物，及其混合物。在优选的实施方案中，在甘油或含甘油，更优选含2至90wt％甘油的增塑剂的混合物存在下，使淀粉变性。优选地，根据本发明的变性或交联淀粉包括相对于淀粉重量，1至40wt％增塑剂。
若存在的话，则组合物内的淀粉优选以具有圆形或椭圆形截面或者在任何情况下截面类似于椭圆的粒子形式存在，且在考虑粒子的主轴情况下测量的其算术平均直径是小于1微米和更优选小于0.5μm的平均直径。
在本发明的优选实施方案中，填充剂是以中值直径小于3微米，优选小于2.5微米,更优选小于2微米的粒子形式存在的矿物填料，更优选是滑石，其中根据ISO 13317-3，通过Sedigraph测量粒度分布。事实上已发现以上所述类型的填充剂的特征在于所述中值直径改进崩解性能以及耐热性和机械性能。优选地，热成形制品的特征在于通过动态机械-扭矩分析(DMTA)，在70℃下获得的G′模量值高于180，优选高于230MPa，和通过DMTA在90℃下获得的G′模量值高于125，优选高于150MPa。
在没有束缚于任何具体理论的情况下，感觉所述填充剂，当在本发明组合物中使用时，在模塑段期间将分层并聚集，进而减慢负责热成形制品崩解的该试剂的作用。
除了组分i.-iv.以外，根据本发明的组合物优选还含有选自下述中的至少一种其他组分：交联剂和/或扩链剂，增塑剂，UV稳定剂，润滑剂，成核剂，表面活性剂，抗静电剂，颜料，阻燃剂，增容剂，木质素，有机酸，抗氧化剂，防霉剂，蜡，加工助剂和优选选自乙烯基聚合物，不是聚酯i.的二酸二醇聚酯，聚酰胺，聚氨酯，聚醚，聚脲和聚碳酸酯中的聚合物组分。
交联剂和/或扩链剂选自具有掺入异氰酸酯，过氧化物，碳二亚胺，异氰脲酸酯，噁唑啉，环氧，酸酐或二乙烯基醚基及其混合物的二-和/或多个官能团的化合物。
优选地，交联剂和/或扩链剂包括具有含异氰酸酯基的二-和/或多个官能团的至少一种化合物。更优选，交联剂和/或扩链剂包括至少25wt％具有掺入异氰酸酯基的二-和/或多个官能团的一种或多种化合物。尤其优选的是具有掺入异氰酸酯基的二-和/或多个官能团的化合物，与具有掺入环氧基的二-和/或多个官能团的化合物，甚至更优选包括至少75wt％具有掺入异氰酸酯基的二-和/或多个官能团的化合物的混合物。
具有掺入异氰酸酯基的二-和多官能团的化合物优选选自对苯二异氰酸酯，2,4-甲苯二异氰酸酯，2,6-甲苯二异氰酸酯，4,4-二苯基甲烷二异氰酸酯，1,3-亚苯基-4-氯二异氰酸酯，1,5-萘二异氰酸酯，4,4-二亚苯基二异氰酸酯，3,3′-二甲基-4,4-二苯基甲烷二异氰酸酯，3-甲基-4,4′-二苯基甲烷二异氰酸酯，二苯基酯二异氰酸酯，2,4-环己烷二异氰酸酯，2,3-环己烷二异氰酸酯，1-甲基2,4-环己基二异氰酸酯，1-甲基2,6-环己基二异氰酸酯，双-(环己基异氰酸酯基)甲烷，2,4,6-甲苯三异氰酸酯，2,4,4-二苯基醚三异氰酸酯，多亚甲基-多苯基-多异氰酸酯，亚甲基二苯基二异氰酸酯，三苯基甲烷三异氰酸酯，3,3′二甲代亚苯基-4,4-二异氰酸酯，4,4′-亚甲基双(2-甲基-苯基异氰酸酯)，六亚甲基二异氰酸酯，1,3-环亚己基二异氰酸酯，1,2-环亚己基二异氰酸酯及其混合物。在优选的实施方案中，含异氰酸酯基的化合物是4,4-二苯基甲烷二异氰酸酯。
关于具有掺入过氧化物基团的二-和多官能团的化合物，这些优选选自过氧化苯甲酰，过氧化月桂酰，过氧化异壬酰，二-(叔丁基过氧异丙基)苯，过氧化叔丁基，过氧化二枯基，α,α′-二(叔丁基过氧)二异丙基苯，2,5-二甲基-2,5二(叔丁基过氧)己烷，过氧化叔丁基枯基，过氧化二叔丁基，2,5-二甲基-2,5-二(叔丁基过氧)己-3-炔，二(4-叔丁基环己基)过氧二碳酸酯，二鲸蜡基过氧二碳酸酯，二肉豆蔻基过氧二碳酸酯，3,6,9-三乙基-3,6,9-三甲基-1,4,7-三过氧壬烷，二(2-乙基己基)过氧二碳酸酯及其混合物。
在根据本发明的组合物中可有利地使用的具有掺入环氧基的二-和多官能团的化合物的实例全部是来自环氧化油的多环氧化物和/或苯乙烯-缩水甘油醚-甲基丙烯酸甲酯，缩水甘油醚甲基丙烯酸甲酯，其包括分子量范围为1000至10000，且每一分子的环氧值范围为1至30，和优选5至25，和选自下述中的环氧化物：二乙二醇二缩水甘油醚，聚乙二醇二缩水甘油醚，甘油聚缩水甘油醚，二甘油聚缩水甘油醚，1,2-环氧基丁烷，聚甘油聚缩水甘油醚，异戊二烯二环氧基和脂环族二环氧化物，1,4-环己烷二甲醇二缩水甘油醚，缩水甘油基2-甲基苯基醚，甘油丙氧基三缩水甘油醚，1,4-丁二醇二缩水甘油醚，山梨醇聚缩水甘油醚，甘油二缩水甘油醚，间二甲苯二胺的四缩水甘油醚，和双酚A的二缩水甘油醚，及其混合物。
与根据本发明组合物的具有掺入异氰酸酯、过氧化物、碳二亚胺、异氰脲酸酯、噁唑啉、环氧基、酸酐和二乙烯基醚基的二-和多官能团的化合物一起，也可使用催化剂，以增加反应性基团的反应性。在聚环氧化物情况下，优选使用脂肪酸的盐，甚至更优选硬脂酸钙和锌。
在本发明尤其优选的实施方案中，组合物中的交联剂和/或扩链剂包括掺入异氰酸酯基的化合物，优选4,4-二苯基甲烷-二异氰酸酯，和/或掺入碳二亚胺基，和/或掺入环氧基的化合物，优选苯乙烯-缩水甘油醚-甲基丙烯酸甲酯类型。
关于增塑剂，除了优选用于制备以上描述的变性淀粉所使用的增塑剂以外，在本发明的组合物中优选存在一种或多种选自苯二甲酸酯类，例如邻苯二甲酸二异壬酯，偏苯三酸酯，例如偏苯三酸与C4-C20一元醇(其优选选自正辛醇和正癸醇)的酯，和具有下述结构的脂族酯中的增塑剂：
R1-O-C(O)-R4-C(O)-[-O-R2-O-C(O)-R5-C(O)-]m-O-R3
其中：
R1选自如下的一种或多种：H，C1-C24类型的直链和支链饱和与不饱和烷基残基，用C1-C24一元酸酯化的多元醇残基；
R2包括-CH2-C(CH3)2-CH2-和亚烷基C2-C8基，且包括至少50mol％所述-CH2-C(CH3)2-CH2-基；
R3选自如下的一种或多种：H，C1-C24类型的直链和支链饱和与不饱和烷基残基，用C1-C24一元酸酯化的多元醇残基；
R4和R5相同或不同，包括一种或多种C2-C22，优选C2-C11，更优选C4-C9亚烷基，且包括至少50mol％的C7亚烷基。
m是1至20，优选2至10，更优选3至7的数值。优选地，在所述酯中，R1和/或R3中的至少一个基团包括相对于R1和/或R3基团的总量，优选用量≥10mol％，更优选≥20％，甚至更优选≥25mol％用至少一种C1-C24一元酸酯化的多元醇残基，所述一元酸选自硬脂酸，棕榈酸，9-酮基硬脂酸，10-酮基硬脂酸，及其混合物。在意大利专利申请MI2014A000030和PCT申请PCT/EP2015/050336，PCT/EP2015/050338中描述了这类脂族酯的实例。
若存在的话，则所选的增塑剂优选以最多10wt％存在，相对于组合物的总重量。
润滑剂优选选自脂肪酸的酯和金属盐，例如硬脂酸锌，硬脂酸钙，硬脂酸铝，和乙酰基硬脂酸酯。优选根据本发明的组合物包括最多1wt％润滑剂，更优选最多0.5wt％，相对于组合物的总重量。
成核剂的实例包括糖精的钠盐，硅酸钙，苯甲酸钠，钛酸钙，氮化硼，全同立构聚丙烯，低分子量PLA。这些添加剂优选以最多10wt％，和更优选2至6wt％的用量添加，相对于组合物的总重量。
视需要，也可添加颜料，例如二氧化钛，粘土，酞菁铜，二氧化钛，硅酸盐，铁的氧化物和氢氧化物，炭黑和氧化镁。这些添加剂优选最多添加10wt％。
在乙烯基聚合物当中，这些优选是：聚乙烯，聚丙烯，它们的共聚物，聚乙烯醇，聚乙酸乙烯酯，聚乙酸乙基乙烯酯，和聚乙烯乙烯醇，聚苯乙烯，氯化乙烯基聚合物，聚丙烯酸酯。
在氯化乙烯基聚合物当中，除了聚氯乙烯以外，此处这些拟包括聚偏二氯乙烯，聚氯化乙烯，聚(氯乙烯-乙酸乙烯酯)，聚(氯乙烯-乙烯)，聚(乙烯氯-丙烯)，聚(氯乙烯-苯乙烯)，聚(氯乙烯-异丁烯)，和其中聚氯乙烯占大于50mol％的共聚物。所述共聚物可以是无规，嵌段或交替共聚物。
关于根据本发明组合物中的聚酰胺，这些优选选自聚酰胺6和6,6，聚酰胺9和9,9，聚酰胺10和10,10，聚酰胺11和11,11，聚酰胺12和12,12，它们中6/9，6/10，6/11，6/12类型的组合，它们的混合物，以及无规和嵌段共聚物二者。
优选地，根据本发明组合物的聚碳酸酯选自聚亚烷基碳酸酯，更优选聚亚乙基碳酸酯，聚亚丙基碳酸酯，聚亚丁基碳酸酯，它们的混合物，和共聚物，无规与嵌段共聚物二者。
在聚醚当中，这些优选是选自分子量为70,000至500,000的聚乙二醇，聚丙二醇，聚丁二醇，它们的共聚物和它们的混合物中的那些。
关于不是聚酯i.的二酸二醇的聚酯，这些优选包括：
a)相对于全部二羧酸组分，含下述的二羧酸组分：
a1)20-100mol％由至少一种芳族二羧酸衍生的单元，
a2)0-80mol％由至少一种饱和脂族二羧酸衍生的单元，
a3)0-5mol％由至少一种不饱和脂族二羧酸衍生的单元；
b)相对于全部二醇组分，含下述的二醇组分：
b1)95-100mol％由至少一种饱和脂族二醇衍生的单元；
b2)0-5mol％由至少一种不饱和脂族二醇衍生的单元。
优选地，用于所述聚酯的芳族二羧酸，饱和脂族二羧酸，不饱和脂族二羧酸，饱和脂族二醇和不饱和脂族二醇选自以上针对根据本发明组合物的聚酯(组分i.)描述的那些。
更优选不是聚酯i.的所述二酸-二醇聚酯选自聚(对苯二甲酸乙二醇酯)，聚(对苯二甲酸丙二醇酯)，聚(对苯二甲酸丁二醇酯)，聚(2,5-呋喃二羧酸乙二醇酯)，聚(2,5-呋喃二羧酸丙二醇酯)，聚(2,5-呋喃二羧酸丁二醇酯)，和聚(2,5-呋喃二羧酸亚烷基酯-共-对苯二甲酸亚烷基酯)类型的嵌段或无规共聚物。
可通过本领域已知的任何方法，进行根据本发明的聚合物组合物的生产方法。有利地，借助挤出工艺生产根据本发明的组合物，其中在熔融状态下混合聚合物组分。在挤出组合物中，各组分可全部一起进料，或者可沿着挤出机独立地进料它们中的一种或多种。
本发明还涉及包括所述聚合物组合物的热成形制品，其中事实上所述聚合物组合物具有可加工性和使得它尤其适合于这一用途的使用性能表现。事实上它的性能使得可制造具有良好的抗变形性，高的尺寸稳定性和在负载下的弯曲温度性能的热成形制品，它能在工业堆肥工艺中崩解和生物降解。优选地，根据EN 13432，包含本发明组合物的热成形制品是可生物降解的，当厚度为最多250μm时。
例如，根据本发明的聚合物组合物尤其适合于制造热成形制品例如板和杯子，硬质容器，用于分配饮料，优选热饮的小容器，盖子和覆盖物，和可在常规与微波烘箱中加热的食品包装。
根据本发明的组合物和包括它的热成形制品优选特征在于低于10mg/kg，优选<5mg/kg的THF含量，且能在与食品接触中使用，正例如在用于分配饮料的小容器情况中发生的一样。
在优选的实施方案中，本发明涉及分配饮料的小容器，其特征在于低于3mg/kg，优选1mg/kg的THF含量。在包括含二羧酸1,4-丁二醇酯单元的聚酯作为组分i.的组合物情况下，可通过对根据本发明的组合物或包含它们的热成形制品进行至少一段THF挥发，从而获得所述低THF含量。
在本发明的优选实施方案中，所述热成形制品包括含本发明组合物的至少一层A以及含选自二酸-二醇聚酯和羟基酸聚酯中的至少一种聚合物的至少一层B，且优选特征在于选自A/B，A/B/A和B/A/B中的所述层A和B的相互排列。在进一步尤其优选的实施方案中，所述层B由乳酸的聚酯组成。
关于借助热成形模塑的方法，可借助本领域技术人员已知的方法，在压力下或者在真空下，由例如片材或膜，热成形本发明的聚合物组合物。本发明还涉及借助热成形，生产模塑制品所使用的含本发明组合物的所述片材或膜。
热成形的典型操作条件提供例如5-8秒的时间加热所述片材或膜，直到它们软化，和模塑时间为15至20秒。
现通过许多实施方案，阐述本发明，所述实施方案拟作为实例且并不限制本专利申请的保护范围。
实施例
组分i
i-1＝根据下述方法制备的聚(琥珀酸1,4-丁二醇酯)("PBS")：在二醇/二羧酸(MGR)的摩尔比为1.08下，将17150g琥珀酸，14000g的1,4-丁二醇，26.75g甘油和2.0g的二异丙基三乙醇胺钛酸酯的80wt％乙醇溶液(Tyzor TE，其含有8.2wt％钛)加入到几何容量为40升的钢反应器中，所述钢反应器配有机械搅拌系统，氮气入口，蒸馏塔，用于高沸点组分的可拆卸系统与高真空系统的连接件。物料的温度在120分钟的时间段内逐渐升高到230℃。当95％的理论水被蒸馏掉时，添加21.25g钛酸四正丁酯(对应于119ppm金属，相对于聚琥珀酸1,4-丁二醇酯的用量(这是将进料到反应器中的所有琥珀酸转化可获得的理论量))。然后升高反应器的温度到235-240℃并在60分钟的时间段内逐渐降低压力到低于2mbar的数值。允许反应进行获得MFR为约7(g/10分钟，在190℃和2.16kg下)的聚(1,4-1,4-丁二醇琥珀酸酯)所要求的时间，然后以长丝形式将材料排放到水浴中并造粒。
i-2＝根据下述方法制备聚(癸二酸1,4-丁二醇酯-共-对苯二甲酸1,4-丁二醇酯)("PBST")：在二醇/二羧酸的摩尔比(MGR)为1.20下，将8160g对苯二甲酸，11198g癸二酸，11296g的1,4-丁二醇，14.4g甘油和2.0g的二异丙基三乙醇胺钛酸酯的80wt％乙醇溶液(Tyzor TE，其含有8.2wt％钛)加入到几何容量为40升的钢反应器中，所述钢反应器配有机械搅拌器系统，氮气入口，蒸馏塔，用于高沸点组分的可拆卸系统与高真空系统的连接件。物料的温度在120分钟的时间段内逐渐升高到230℃。当95％的理论水被蒸馏掉时，添加21.2g钛酸四正丁酯(对应于119ppm金属，相对于PBST的用量(这是将进料到反应器中的所有癸二酸和所有对苯二甲酸转化可获得的理论量))。然后升高反应器的温度到235-240℃，并在60分钟的时间段内逐渐降低压力到低于2mbar的数值。允许反应进行获得MFR为约5(g/10分钟，在190℃和2.16kg下)的聚(癸二酸1,4-丁二醇酯-共-对苯二甲酸1,4-丁二醇酯)所要求的时间，然后以长丝形式将材料排放到水浴中并造粒。
组分ii
ii＝Ingeo 4043D聚乳酸("PLA")，MFR 3.5/10min(在190℃，2.16kg下)。
组分iii
iii＝HMV-15CA Carbodilite，获自Nisshinbo Chemical Inc。
组分iv
iv＝中值直径为1.9微米的微米化滑石(根据ISO 13317-3，通过Sedigraph测定粒度分布)，Mistron R10C商业等级，获自Imerys。
实施例1-3-生产含本发明组合物的热成形制品
表1-实施例1-3的组合物
在下述操作条件下，将表1的组合物进料到Icma San Giorgio MCM 25 HT型号的同向旋转的双螺杆挤出机中：
螺杆直径(D)＝25mm；
L/D＝52；
旋转速度＝200rpm；
温度特征曲线＝100-180-215×9-180-170-160℃；
生产量10.1kg/h；
在真空下脱气；
将粒子进料到配有扁平头400mm宽以及3个400宽度和200直径的辊的Teknomast配混辊压单元并提供有水冷的Curti单螺杆挤出机(螺杆直径40mm-L/D25)中。操作条件如下所述：
螺杆直径(D)＝40mm；
L/D＝25；
旋转速度＝60rpm；
温度特征曲线＝挤出机：190-5×200℃/头：6×200℃；
生产量20kg/h。
由片材获得棒状物(长度30mm，宽度6mm，厚度0.5mm)，然后在扭矩模式下，使用获自TA Instrument的Ares G2旋转流变仪，经历动态机械-扭矩分析(DMTA)。强加0.1％的变形和1Hz的频率，在3℃/min下从30℃加热样品到120℃。
根据标准ASTM-D648，使用0.455MPa负载(方法B)，在"棒状物"类型的模塑试样(长度127mm，宽度12.7mm，厚度3.2mm)上，使用Ceast 6510 Test-A-Matic型号设备，测量热偏移温度(HDT)。对于每一组合物，三次测定HDT值。所描述的值对应于所测量值的算术平均。
在Artpack热成形机上，在生产板的单一模头的模具(直径220mm，深度40mm)中，使用下述热成形操作条件，热成形厚度为350μm的片材：
-通过15 IR灯加热(每一盏灯的额定最大功率为325W)；
-加热时间5-8秒(至软化)；
-总的循环时间15-20秒。
在根据标准ISO20200:2004的控制堆肥中，所得板经历崩解试验，从而显示出在58℃下超过90天重量损失大于90％。
表2-HDT和DMTA表征
| 实施例 | HDT℃ | G′[MPa]a T＝70℃ | G′[MPa]a T＝90℃ |
| 1 | 91±1 | 340 | 232 |
| 2 | 82±1 | 309 | 202 |
| 3 | 82±1 | 271 | 176 |
Claims (13)
1.用于生产热成形制品的聚合物组合物，所述聚合物组合物包含，相对于组分i.-iv.之和：
i)20-60wt％至少一种聚酯i.，所述聚酯包括：
a)二羧酸组分，所述二羧酸组分相对于全部二羧酸组分包含：
a1)0-20mol％由至少一种芳族二羧酸衍生的单元，
a2)80-100mol％由至少一种饱和脂族二羧酸衍生的单元，
a3)0-5mol％由至少一种不饱和脂族二羧酸衍生的单元；
b)二醇组分，所述二醇组分相对于全部二醇组分包含：
b1)95-100mol％由至少一种饱和脂族二醇衍生的单元；
b2)0-5mol％由至少一种不饱和脂族二醇衍生的单元；
ii)5-35wt％至少一种聚羟基烷酸酯ii.；
iii)0.01-5wt％的至少一种水解稳定剂，所述水解稳定剂包含具有二-和/或多个官能团的至少一种化合物，该官能团包括碳二亚胺基团；
iv)5-50wt％至少一种填充剂。
2.权利要求1的聚合物组合物，其中所述至少一种聚酯i.包括脂族聚酯(AP)，所述脂族聚酯包括二羧酸组分和二醇组分，所述二羧酸组分由相对于二羧酸组分的总摩尔数，95-100mol％由至少一种饱和脂族二羧酸衍生的单元和0-5mol％由至少一种不饱和脂族二羧酸衍生的单元组成，和所述二醇组分包括相对于二醇组分的总摩尔数，95-100mol％由至少一种饱和脂族二醇衍生的单元和0-5mol％由至少一种不饱和脂族二醇衍生的单元。
3.权利要求2的聚合物组合物、其中所述脂族聚酯(AP)选自聚(琥珀酸1,4-丁二醇酯)、聚(己二酸1,4-丁二醇酯)、聚(壬二酸1,4-丁二醇酯)、聚(癸二酸1,4-丁二醇酯)、聚(己二酸1,4-丁二醇酯-共-琥珀酸1,4-丁二醇酯)、聚(壬二酸1,4-丁二醇酯-共-琥珀酸1,4-丁二醇酯)、聚(癸二酸1,4-丁二醇酯-共-琥珀酸1,4-丁二醇酯)、聚(琥珀酸1,4-丁二醇酯-共-己二酸1,4-丁二醇酯-共-壬二酸1,4-丁二醇酯)。
4.权利要求2和3任何一项的聚合物组合物，其中所述脂族聚酯(AP)是聚(琥珀酸1,4-丁二醇酯)。
5.权利要求1-4任何一项的聚合物组合物，其中所述至少一种聚羟基烷酸酯ii.选自乳酸的聚酯、聚-ε-己内酯、聚羟基丁酸酯、聚羟基丁酸酯-戊酸酯、聚羟基丁酸酯丙酸酯、聚羟基丁酸酯己酸酯、聚羟基丁酸酯癸酸酯、聚羟基丁酸酯十二烷酸酯、聚羟基丁酸酯-十六烷酸酯、聚羟基丁酸酯-十八烷酸酯、聚-3-羟基丁酸酯4-羟基丁酸酯。
6.权利要求1-5任何一项的聚合物组合物，其中在水解稳定剂iii.中使用的所述具有掺入碳二亚胺基团的二-和多个官能团的至少一种化合物选自聚(亚环辛基碳二亚胺)，聚(1,4-二亚甲基亚环己基碳二亚胺)，聚(二环己基甲烷碳二亚胺)，聚(亚环己基碳二亚胺)，聚(亚乙基碳二亚胺)，聚(亚丁基碳二亚胺)，聚(亚异丁基碳二亚胺)，聚(亚壬基碳二亚胺)，聚(亚十二烷基碳二亚胺)，聚(亚新戊基碳二亚胺)，聚(1,4-二亚甲基亚苯基碳二亚胺)，聚(2,2′,6,6′-四异丙基二亚苯基碳二亚胺)(D)，聚(2,4,6-三异丙基-1,3-亚苯基碳二亚胺)(P-100)，聚(2,6二异丙基-1,3-亚苯基碳二亚胺)(P)，聚(甲苯基碳二亚胺)，聚(4,4′-二苯基甲烷碳二亚胺)，聚(3,3′-二甲基-4,4′-亚联苯基碳二亚胺)，聚(对亚苯基碳二亚胺)，聚(间亚苯基碳二亚胺)，聚(3,3′-二甲基-4,4′-二苯基甲烷碳二亚胺)，聚(亚萘基碳二亚胺)，聚(异佛尔酮碳二亚胺)，聚(枯烯碳二亚胺)，对亚苯基双(乙基碳二亚胺)，1,6-六亚甲基双(乙基碳二亚胺)，1,8-八亚甲基双(乙基碳二亚胺)，1,10-十亚甲基双(乙基碳二亚胺)，1,12-十二亚甲基双(乙基碳二亚胺)及其混合物。
7.权利要求1-6任何一项的聚合物组合物，其中所述至少一种填充剂iv.是矿物填料。
8.权利要求7的聚合物组合物，其中所述至少一种填充剂iv.是滑石。
9.权利要求7和8任何一项的聚合物组合物，其中所述滑石以中值直径小于3微米的粒子形式存在。
10.权利要求7和8任何一项的聚合物组合物，其中所述滑石以中值直径小于2.5微米的粒子形式存在。
11.权利要求7和8任何一项的聚合物组合物，其中所述滑石以中值直径小于2微米的粒子形式存在。
12.一种热成形制品，包括权利要求1-11任何一项的聚合物组合物。
13.权利要求12的热成形制品，其选自板、杯子、硬质容器、用于分配饮料的小容器、盖子、覆盖物、或可在常规或微波烘箱中加热的用于食品的容器。
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| CN109762314A (zh) * | 2019-01-14 | 2019-05-17 | 温州信环生物材料科技有限公司 | 一种可生物降解的发泡材料及利用其制造耐热发泡餐盒的方法 |
| CN111499849A (zh) * | 2020-05-29 | 2020-08-07 | 陕西科技大学 | 一种多羟基亲水性可生物降解材料及其制备方法和应用 |
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