CN102459070A - 改善了安全性的高氯酸盐溶液、以及用于使含氯树脂组合物热稳定的方法 - Google Patents
改善了安全性的高氯酸盐溶液、以及用于使含氯树脂组合物热稳定的方法 Download PDFInfo
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- CN102459070A CN102459070A CN2010800317952A CN201080031795A CN102459070A CN 102459070 A CN102459070 A CN 102459070A CN 2010800317952 A CN2010800317952 A CN 2010800317952A CN 201080031795 A CN201080031795 A CN 201080031795A CN 102459070 A CN102459070 A CN 102459070A
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- chlorine
- water
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- 239000003960 organic solvent Substances 0.000 claims abstract description 17
- 229910052751 metal Inorganic materials 0.000 claims abstract description 15
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- C01B11/00—Oxides or oxyacids of halogens; Salts thereof
- C01B11/16—Perchloric acid
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Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
为了改善用作含氯树脂稳定剂的高氯酸盐溶液的操作性和安全性。本发明提供了具有改善的操作性和安全性的高氯酸盐溶液，以及通过向100重量份的含氯树脂中加入以下物质来使含氯树脂组合物热稳定的方法：(a)0.004-10重量份的高氯酸盐溶液，所述高氯酸盐溶液含有1-60重量％的高氯酸盐、5-50重量％的水溶性有机溶剂、以及20-94重量％的水；和(b)0.001-10重量份的至少一种由通式(I)M(O)a nSiO2mH2O表示的硅酸盐化合物，在通式(I)中，M是至少一种选自碱土金属和铝的金属，当M为碱土金属时a为1，当M为铝时a为3/2，n是1-5，且m是任意正整数。
Description
技术领域
本发明涉及用于改善作为含氯树脂(如PVC)用稳定剂助剂的高氯酸盐溶液的加工性或操作性和安全性的方法。
本发明还涉及高氯酸盐溶液与稳定剂一起用于含氯树脂以改善稳定剂的操作性和安全性的用途。
本发明进一步涉及用于使含氯树脂组合物热稳定的方法。
背景技术
含氯树脂(如聚氯乙烯(PVC))具有多种优异的性能并用于宽范围的应用。但是，它们具有这样的缺点：当它们经历热模塑技术时，它们由于脱氯化氢而降解，使得所得的模塑制品变色，从而损害产品价值。
为了改善含氯树脂的热稳定性，已向含氯树脂中加入多种稳定剂。存在几种类型的稳定剂，包括铅基体系、有机锡体系和金属皂基体系。
最近，含有含氯树脂(如PVC)的组合物广泛地用作用于模制汽车内部装饰部件的材料。具体地说，它们的用途扩大至用于缓冲垫、扶手、头靠、控制台、仪表盖、门边等的覆盖材料。在这样的作为用于车辆内部装饰部件的覆盖材料的应用中，通常的实践是：在由含有含氯树脂的组合物形成的层的背侧上通过粘附或注射来形成聚氨酯泡沫层，从而改善内部装饰部件的回弹性和触感。粉末旋转模塑技术或粉末搪塑技术(powder-slush mouldingtechnique)最近也用于模制车辆内部装饰部件。
在车辆内部装饰部件的情况中，它们需要具有这样的性质或性能：它们可以令人满意地经受住较长持续时间地暴露于70℃到140℃的温度的恶劣条件，其中，所述持续时间取决于预期的应用。长时间处于这样的高温条件下，包含含氯树脂组合物层和通过粘附或注射结合到该含氯树脂组合物层的聚氨酯层的复合材料将变色或物理劣化，从而严重损害车辆内部装饰部件的品质性能和产品价值。实际上，据认为，由聚氨酯泡沫的热降解产生的残留胺化合物和氰化物可迁移到含氯树脂组合物层中，导致促进含氯树脂组合物层的热降解。
为了克服上述技术问题，已经提出向含氯树脂组合物中加入键合至有机基团的有机金属盐化合物(金属皂)与溶于有机溶剂中的高氯酸盐溶液或者与高氯酸盐水溶液的组合作为稳定剂(参见下述专利文献No.1～No.6)。
专利文献No.1：JP-B1-57-57056
专利文献No.2：JP-B1-57-47925
专利文献No.3：JP-B1-57-47926
专利文献No.4：JP-B1-57-47927
专利文献No.5：JP-B1-63-462
专利文献No.6：JP-U1-58-122951
但是，当有机溶剂大量用于稳定剂时，它们在车辆内部蒸发，导致起雾、发臭气以及乘客健康的问题。另一方面，当使用高氯酸盐的水溶液时，通过水从高氯酸盐水溶液蒸发而导致在工厂中的管线内形成高氯酸盐晶体，从而存在由高氯酸盐晶体的摩擦或撞击而导致的爆炸或起火的危险。
因此，需要提供具有改善的操作性和安全性且不损害高氯酸盐的作用的高氯酸盐使用方法。
发明内容
所要解决的技术问题
本发明的目的是通过使用具有高沸点的水溶性有机溶剂和水的混合物来制备高氯酸盐溶液以改善用作含氯树脂稳定剂的高氯酸盐溶液的操作性和安全性。
解决技术问题的技术方案
本发明提供用于含氯树脂稳定剂的高氯酸盐溶液，其包含1-60重量％的高氯酸盐、5-50重量％的水溶性有机溶剂、以及20-94重量％的水。
本发明的有益效果
通过使用根据本发明的具有改善的操作性和安全性的高氯酸盐溶液，在包含高氯酸盐的含氯树脂组合物的生产期间，操作性能和安全性可被改善。根据本发明的使含氯树脂组合物热稳定的方法对于通过粉末模塑技术生产基于氯乙烯的树脂组合物是有效的，其中，所述粉末模塑技术在热稳定性、热老化和变色方面是优越的。
具体实施方式
所述水溶性有机溶剂优选具有高于150℃且最优选高于200℃的沸点。如果使用沸点低于150℃的溶剂，抑制高氯酸盐结晶化的作用将不令人满意。
所述水溶性有机溶剂的例子包括乙二醇、乙二醇单丁醚、乙二醇单异戊醚、乙二醇单苯醚、乙二醇单苄醚、乙二醇单己醚、二甘醇、二甘醇单甲醚、二甘醇单丁醚、醋酸二甘醇酯、三甘醇、三甘醇单甲醚、三甘醇单乙醚、三甘醇单丁醚、四亚甲基二醇、聚乙二醇、丙二醇、丙二醇单丁醚、一缩二丙二醇、一缩二丙二醇单甲醚、一缩二丙二醇单乙醚、二缩三丙二醇、二缩三丙二醇单甲醚、1，4-丁二醇、1，5-戊二醇、己二醇、辛二醇、甘油、单醋酸甘油酯、二醋酸甘油酯和单丁酸甘油酯。这些溶剂在本发明中可单独使用或可使用多种类型的混合物。
根据本发明的用于含氯树脂稳定剂的高氯酸盐溶液通过使用下述混合物(总计为100重量％)来制备：
1-60重量％的高氯酸盐，
5-50重量％的水溶性有机溶剂，和
20-94重量％的水。
高氯酸盐溶液可与其它稳定剂和/或稳定剂助剂一起使用。根据本发明的高氯酸盐溶液的量通常在0.01-10重量份、优选0.05-5重量份的范围内，相对于100重量份的含氯树脂。
作为用于本发明的其它稳定剂，可以是：从钡/锌体系和钙/锌体系的金属苯酚盐和金属羧酸盐开始的有机金属盐；基于酚类或硫的抗氧化剂；有机亚磷酸酯化合物；紫外线吸收剂；基于受阻胺的光稳定剂；早期变色抑制剂(early-colouration inhibitor)；有机锡化合物；以及环氧化合物。
用于本发明的高氯酸盐可以是高氯酸化(perchloric)的锂、钠、钾、锶、钡、锌、铝和铵盐。这些可以是无水或水合的盐，且它们可以单独使用或以混合物的形式使用。
当高氯酸盐用作用于含氯树脂组合物的稳定剂时，相对于100重量份的含氯树脂，这通过加入以下物质而完成：
(a)0.004-10重量份的高氯酸盐溶液，所述高氯酸盐溶液含有1-60重量％的高氯酸盐、5-50重量％的水溶性有机溶剂、以及20-94重量％的水；和
(b)0.001-10重量份的至少一种由通式(I)表示的硅酸盐化合物：
M(O)a nSiO2mH2O (I)
在通式(I)中，M是至少一种选自碱土金属和铝的金属，当M为碱土金属时a为1，当M为铝时a为3/2，n是1-5，且m是任意正整数。
在本发明中，含氯树脂组合物的稳定化可以通过进一步添加0.05-10重量份的由通式(II)表示的水滑石来更有效地实现：
M(1-x)Alx(OH)2(An- x/n)mH2O (II)
在通式(II)中，M表示Mg和/或Zn，An-表示CO3 2-和/或ClO4 -的n价阴离子，x是0＜x＜0.5，且m在0≤m＜3的范围内。
存在天然和合成形式的上述水滑石化合物，并且两者均可用于本发明。
另外，还可以使用其表面上已覆盖有以下物质的那些：高级脂肪酸，如硬脂酸或油酸；高级脂肪酸的金属盐；有机磺酸金属盐，如十二烷基苯磺酸的碱金属盐；高级脂肪酸酯；高级脂肪酸酰胺；蜡；或高氯酸等。
前述有机金属盐的金属可以是钠、钾、锂、镁、钙、钡、锌和铝。
有机酸残基可以是羧酸、苯酚或烷基酚(例如下面所示的那些)的残基。
羧酸是具有1-22个碳原子的饱和或不饱和的脂族羧酸、具有7-16个碳原子的环状或杂环羧酸、以及具有2-10个碳原子的羟基酸或烷氧基酸，并且实际例子包括甲酸、乙酸、丙酸、羊脂酸、辛酸、2-乙基己酸、新癸酸、异癸酸、月桂酸、硬脂酸、肉豆蔻酸、棕榈酸、山萮酸、环氧化硬脂酸、异硬脂酸、12-羟基硬脂酸、12-酮硬脂酸、油酸、蓖麻油酸、罂酸(linolic acid)、亚油酸(linoleic acid)、羟基乙酸、乳酸、氢化丙烯酸(hydroacrylic acid)、α-氧代乙酸、甘油酸(glycerolic acid)、苹果酸、酒石酸、柠檬酸、巯基乙酸、巯基丙酸、月桂基巯基丙酸、苯甲酸、对叔丁基苯甲酸、甲苯酸、二甲基苯甲酸、氨基苯甲酸、水杨酸、氨基乙酸、谷氨酸、草酸、丁二酸、己二酸、邻苯二甲酸、马来酸和硫代二丙酸。
苯酚和烷基酚的例子包括苯酚、壬基酚、十二烷基苯酚、叔丁基苯酚、辛基酚、异戊基酚和甲酚。
这些羧酸的金属盐和烷基酚的金属盐可以是酸式盐或中性盐，或者它们可以是碱式盐、碳酸盐或过碱式盐(per-basic salt)。
此外，这些有机金属盐的添加量是0.1-10重量份、且优选0.2-5重量份，相对于100重量份的含氯树脂。可使用这些金属盐的一种，或者两种或更多种类型的混合物。
前述有机锡化合物可以是，例如，二甲基氧化锡、二丁基氧化锡、二辛基氧化锡、二甲基硫化锡、二丁基硫化锡、二辛基硫化锡、二丁基锡二月桂酸酯、二丁基锡二硬脂酸酯、二辛基锡二油酸酯、二辛基锡二月桂酸酯、二辛基锡二硬脂酸酯、二辛基锡双(油烯基苹果酸酯)、二丁基锡(硬脂基苹果酸酯)、二丁基锡苹果酸酯聚合物、二辛基锡苹果酸酯聚合物、二辛基锡双(丁基苹果酸酯)、二丁基锡β-巯基丙酸酯、二辛基锡β-巯基丙酸酯、二丁基锡巯基乙酸酯、单丁基锡三(2-乙基己基巯基乙酸酯)、二丁基锡双(2-乙基己基巯基乙酸酯)、单辛基锡三(2-乙基己基巯基乙酸酯)、二丁基锡(异辛基巯基乙酸酯)、二辛基锡双(异辛基巯基乙酸酯)、二辛基锡双(2-乙基己基巯基乙酸酯)、二甲基锡双(异辛基巯基丙酸酯)、单丁基锡三(异辛基巯基丙酸酯)和单辛基锡三(异辛基巯基丙酸酯)。
这些有机锡化合物的添加量是0.01-10重量份、且优选0.05-5重量份，相对于100重量份的含氯树脂。
前述早期变色抑制剂可以是β-二酮化合物和环丁砜化合物。
β-二酮化合物是，例如，脱氢乙酸、环己烷-1，3-二酮、2-苯甲酰基环戊酮、2-乙酰基环己酮、2-苯甲酰基环己酮、乙酰基硬脂酰甲烷、苯甲酰基丙酮、棕榈酰基苯甲酰甲烷、硬脂酰基苯甲酰甲烷、二苯甲酰基甲烷、三苯甲酰基甲烷、4-甲氧基苯甲酰苯甲酰甲烷、双(4-甲氧基苯甲酰甲烷)、4-氯苯甲酰苯甲酰甲烷、苯甲酰基三氟丙酮、棕榈酰基四氢萘酮、硬脂酰基四氢萘酮和苯甲酰基四氢萘酮。
前述β-二酮化合物可以是金属络合物盐，而且，形成所述络合物盐的金属是钠、钙和钡或锌。
这些早期变色抑制剂的添加量是0.0005-10重量份、且优选0.001-5重量份，相对于100重量份的含氯树脂。可使用这些早期变色抑制剂中的一种、或者两种或更多种类型的混合物。
前述有机亚磷酸酯化合物的代表为三烷基亚磷酸酯、三芳基亚磷酸酯、烷基芳基亚磷酸酯、双酚A亚磷酸酯、多元醇亚磷酸酯、以及其中一个或多个有机酯残基被氢原子取代的酸式亚磷酸酯，而且，这样的亚磷酸酯化合物的例子包括亚磷酸三苯酯、三异辛基亚磷酸酯、三异癸基亚磷酸酯、三异十二烷基亚磷酸酯、三异十三烷基硫代亚磷酸酯、二苯基异辛基亚磷酸酯、二苯基异癸基亚磷酸酯、二苯基十三烷基亚磷酸酯、二异癸基季戊四醇二亚磷酸酯、四苯基一缩二丙二醇二亚磷酸酯、聚(一缩二丙二醇)苯基亚磷酸酯、三月桂基硫代亚磷酸酯、二硬脂基季戊四醇二亚磷酸酯、三-2，4-二-叔丁基苯基亚磷酸酯、2，4-二-叔丁基苯基二异癸基亚磷酸酯、三丁氧基乙基亚磷酸酯、4，4′-异亚丙基二苯基烷基(C12到C15)二亚磷酸酯和五(一缩二丙二醇)三亚磷酸酯、4，4′-亚丁基双(3-甲基-6-叔丁基-二-十三烷基亚磷酸酯)。
此外，其中前述亚磷酸酯化合物中的一个或两个有机残基被氢原子取代的酸式亚磷酸酯也是有效的，而且，这些的例子包括二苯基酸式亚磷酸酯、单苯基酸式亚磷酸酯、二异辛基酸式亚磷酸酯、单异辛基酸式亚磷酸酯、双-十三烷基酸式亚磷酸酯、二苄基酸式亚磷酸酯、二壬基苯基酸式亚磷酸酯等。
此外，前述有机磷酸酯化合物(如壬基苯基聚氧乙烯(5-55)磷酸酯、十三烷基聚氧乙烯(4-10)磷酸酯等)可用作加工助剂。而且，有机磷酸酯的金属加合物(例如，单/双(混合)异辛基磷酸酯的镁、钙、钡或锌盐，单/双(混合)异十三烷基磷酸酯的镁、钙、钡或锌盐等)可分别用作热稳定化助剂。
此外，其中前述有机磷酸酯中的一个或两个有机残基被氢原子取代的酸式磷酸酯也是有效的，而且，例子包括丁基酸式磷酸酯、丁氧基乙基酸式磷酸酯、2-乙基己基酸式磷酸酯和硬脂基酸式磷酸酯。此外，也存在金属盐，例如，这些酸式磷酸酯的镁、钙、钡或锌盐。
前述抗氧化剂是受阻酚，例如，烷基酚、烷基化的苯酚酯、亚烷基和烷叉基的双酚、多烷基化的苯酚酯，而且，这些的例子包括丁羟茴醚、4-羟甲基-2，6-二-叔丁基酚、4，4′-二羟基-2，2′-二苯基丙烷、2，2′-亚甲基双(4-甲基-6-叔丁基酚)、4，4′-硫代双(6-叔丁基-3-甲酚)和四[亚甲基-3(3′，5′-二-叔丁基-4′-羟苯基)丙酸酯基(propionato)]甲烷。
此外，举例来说，还有二月桂基硫代丙酸酯、二硬脂基硫代丙酸酯等作为含硫的链烷酸烷基酯。
前述环氧化合物是环氧化的不饱和的油和脂肪、环氧化的不饱和脂族酸酯、环氧环己烷衍生物、或表氯醇衍生物，而且，例子包括：环氧化大豆油；环氧化蓖麻油；环氧化亚麻子油；环氧化红花籽油；环氧化亚麻子油脂肪酸丁基酯；环氧化的硬脂酸的丁酯、异辛酯、2-乙基己基烷基酯，以及与钙、锌等的金属盐；3-(2-联苯氧基(xenoxy))-1，2-环氧丙烷、环氧六氢邻苯二甲酸二-2-乙基己基酯、环氧聚丁二烯、双酚A二缩水甘油醚等。
其它的稳定剂助剂可以是多元醇，如单和双季戊四醇、甘露糖醇和山梨糖醇，而且，存在羧酸、氨基酸或松香与这些多元醇的酯化合物，如季戊四醇硬脂酸酯、季戊四醇己二酸酯、季戊四醇吡咯烷酮羧酸酯、季戊四醇谷氨酸酯、木松香季戊四醇、季戊四醇马来酸酐木松香酯、和木松香甘油酯。此外，存在基于苯并三唑的化合物(如1，2，3-苯并三唑、甲苯基三唑等)，噻唑化合物(如2-巯基苯并噻唑等)，β-氨基巴豆酸与1，3-或1，4-丁二醇、1，2-一缩二丙二醇、硫代二乙二醇、月桂醇等的酯化合物，以及作为含氮化合物的三(2-羟乙基)异氰酸酯和三(巯基乙基)异氰脲酸酯化合物。
用作前述紫外吸收剂的材料的代表为基于苯并三唑的材料和基于二苯甲酮的材料，而且，例如，存在苯并三唑化合物，如2-(5-甲基-2-羟苯基)苯并三唑、2-(3，5-二-叔丁基-2-羟苯基)-5-氯苯并三唑、和2-(3，5-二-叔戊基-2-羟苯基)苯并三唑、和2，5-二甲基琥珀酸酯-1-(2-羟乙基)-4-羟基-2，2，6，6-四甲基哌啶缩合物作为基于苯并三唑的紫外线吸收剂。例如，存在2，4-二羟基二苯甲酮、2-羟基-4-甲氧基二苯甲酮、2，2′-二羟基-4-甲氧基二苯甲酮、2，2′-二羟基-4，4′-二甲氧基二苯甲酮和2-羟基-4-壬氧基(noctoxy)二苯甲酮作为基于二苯甲酮的紫外线吸收剂。
可以用作前述光稳定剂的物质是，例如，受阻胺化合物，如聚[{6-(1，1，3，3-四甲基丁基)氨基-1，3，5-三嗪-2，4-二基}{(2，2，6，6-四甲基-4-哌啶基)氨基}六亚甲基{(2，2，6，6-四甲基-4-哌啶基)亚氨基}]。
可与本发明产品一起使用的含氯树脂的例子包括：聚氯乙烯；氯化聚氯乙烯；氯乙烯/醋酸乙烯酯共聚物；氯乙烯/乙烯共聚物；氯乙烯/丙烯共聚物；氯乙烯/苯乙烯共聚物；氯乙烯/异丁烯共聚物；氯乙烯/亚乙烯基共聚物；氯乙烯/苯乙烯/马来酸酐三元共聚物；氯乙烯/烷基、环烷基或芳基马来酰亚胺共聚物；氯乙烯/苯乙烯/丙烯腈共聚物；氯乙烯/丁二烯共聚物；氯乙烯/异戊二烯共聚物；氯乙烯/氯化丙烯共聚物；氯乙烯/偏二氯乙烯/醋酸乙烯酯三元共聚物；氯乙烯/丙烯酸酯共聚物；氯乙烯/马来酸酯共聚物；氯乙烯/甲基丙烯酸酯共聚物；氯乙烯/丙烯腈共聚物；氯乙烯/氨基甲酸酯共聚物；聚偏二氯乙烯；氯化聚乙烯；以及氯化聚丙烯。对于树脂的形式或者树脂的聚合或生产方法无具体限定。
在本发明中，根据需要并根据预期目的，可以适当地使用增塑剂、抗静电剂、抗起雾剂、金属钝化剂(如防锈剂等)、杀真菌剂、抗菌剂、积垢(plate-out)抑制剂(如低分子量的丙烯酸酯低聚物脱模剂)、降粘剂、表面活性剂、荧光增白剂、起泡剂、基于丙烯酸类的泡孔控制剂、加工助剂、润滑剂、无机盐或无机金属化合物、以及颜料、填料如碳酸钙、粘土、阻燃剂、表面处理剂、交联剂、增强剂。
前述增塑剂的例子包括：基于邻苯二甲酸酯的增塑剂，如邻苯二甲酸二-2-乙基己基酯、邻苯二甲酸二丁酯、邻苯二甲酸二异癸基酯、二混合烷基(C9～11)邻苯二甲酸酯、邻苯二甲酸二庚酯、邻苯二甲酸二异壬基酯等；基于己二酸酯的增塑剂，如己二酸二-2-乙基己基酯、己二酸二异壬酯、己二酸二异丁酯和己二酸二异癸酯；基于偏苯三酸酯的增塑剂，如偏苯三酸三-2-乙基己基酯、偏苯三酸三-正辛基酯、偏苯三酸三异癸酯、偏苯三酸三丁酯等；基于癸二酸酯的增塑剂，如癸二酸二-2-乙基己基酯、癸二酸二丁酯；以及基于磷酸酯的增塑剂、基于聚酯的增塑剂、基于氯化石蜡的增塑剂、基于均苯四酸酯的增塑剂和基于环氧的增塑剂。
前述无机盐或无机金属化合物具有，例如，金属钠、钾、镁、钙、钡、锌、铝或锡作为金属，而且，存在这些金属的氧化物、氢氧化物、硅酸盐、硼酸盐、硫酸盐、高氯酸盐、亚磷酸盐、磷酸盐、碱式碳酸盐和碱式磷酸盐。
这些化合物可以是络合物盐且它们可以是无水或具有结晶水的水合物，而且，它们可以具有混合物的形式。此外，它们还可以是与多元醇的络合物。
这些化合物的典型实例包括可由(III)表示的含钙氢氧化物、氧化钙、氧化镁、氧化锌、氧化硅、氧化铝、氢氧化钙、氢氧化镁、氢氧化钡、氢氧化铝、硅酸钠、硅酸钙、硅酸锌、硅酸铝、硅酸铝钾、硼酸钠、硼酸钾、硼酸铝、硼酸铝、硫酸铝十八水合物、硫酸铝钠十二水合物、磷酸钠、焦磷酸钠、磷酸镁、磷酸钙、正磷酸钙、正磷酸锌、钠取代的A-型沸石、钙取代的A-型沸石、镁取代的A-型沸石、硅灰石以及雪硅钙石。
Ca(1-x)Mx(OH)2 (III)
其中M表示Mg或Al，且x在0.005＜x＜0.5的范围内。
实施例
现在，本发明基于以下所示的示例性实施例进行更详细地描述。当然，本发明完全不限于这些示例性实施例。
实施例1(制备)
(实施例1-1)
将三甘醇单甲醚(沸点249℃)(10g)与66.7g的60％高氯酸钠水溶液混合，然后，混入23.3g水来制备40％高氯酸钠溶液。
(实施例1-2)
将聚乙二醇200(沸点高于250℃)(10g)与66.7g的60％高氯酸钠水溶液混合，然后，进一步混入23.3g水来制备40％高氯酸钠溶液。
(实施例1-3)
将甘油(沸点290℃)(10g)与66.7g的60％高氯酸钠水溶液混合，然后，进一步混入23.3g水来制备40％高氯酸钠溶液。
(实施例1-4)
将甘油(沸点290℃)(20g)与66.7g的60％高氯酸钠水溶液混合，然后，进一步混入13.3g水来制备40％高氯酸钠溶液。
将前述实施例中所制备的各稳定剂组分(10.0g)分别在皮氏培养皿(直径约60mm)中称重，并在室温下以敞开状态静置10天，观察水组分蒸发和晶体沉淀的情况。
评价标准
对于由蒸发导致的失重，以10天中的重量下降的比例(％)来表示，而且，对于晶体沉淀，以在10天中观察到沉淀的那一天来表示。
(对比例1-1)
将水(33.3g)与66.7g的60％高氯酸钠水溶液混合来制备40％高氯酸钠溶液。
(对比例1-2)
将丙二醇单甲醚(熔点120℃)(10g)与66.7g的60％高氯酸钠水溶液混合，然后，进一步混入23.3g水来制备40％高氯酸钠溶液。
表1
*：到第10天几乎蒸干
从上表1显见，由于高氯酸钠水溶液(对比例1-1)和其中已加入低沸点有机溶剂的高氯酸钠水溶液(对比例1-2)的水的蒸发，易于沉淀出晶体，而且，它们的操作是危险的，但是，当包含高沸点的水溶性有机溶剂(实施例1-1至1-4)时，抑制了晶体的沉淀。
对于实施例1-4，在10天内无晶体沉淀。抑制了晶体的沉淀并避免了由于由干燥导致的结晶材料的飞散而产生的污染事故，而且，材料可被安全地处理。
实施例2(聚氨酯衬板(Polyurethane-lined sheet))
按照以下所示的配方，将在各前述制备实施例中制备的稳定剂组分加入到氯乙烯树脂组合物中。
将所述氯乙烯树脂组合物在吉尔(Geer)烘箱中在110℃干燥1小时，然后，通过使用破碎机混合5分钟来制得配混料。使用这些配混料，以下述粉末模塑技术制得板材。在300℃的吉尔烘箱中，将铬镜面板加热到超过240℃约15分钟。
从吉尔烘箱中取出所述板，并且，当所述镜面板达到240℃时，将所述配混料喷撒到该板上，使所述配混料迅速展开至均匀厚度并静置10秒。
清除未胶凝的过量配混料，然后，将其置于350℃的电烘箱中15秒并完全胶凝。取出模具并冷却，得到板材。
聚氨酯衬板的测试
将前述获得的板材置于模具中，然后，将多元醇(EP-3033，MitsuiChemical Polyurethane Co.，Ltd)和多异氰酸酯(CR-200，Mitsui ChemicalPolyurethane Co.，Ltd)(重量比10∶7)(参见下述配方)的聚氨酯液态混合物注入到该模具中，以生产PVC板+厚度20mm的聚氨酯泡沫体的复合材料。
注释*：TEDA(三亚乙基二胺，Kantou Chemical)和三乙醇胺(KantouChemical)是催化剂。
将所得的聚氨酯衬板在120℃的烘箱中加热500小时，然后，通过观察颜色变化ΔE来评价稳定性。标准如下：
10分 高于ΔE20，黑色分解
0分 低于ΔE2
结果示于表2中。
表2
| 高氯酸盐溶液 | PUF衬板样品的热老化性质 | |
| 实施例2-1 | 无 | 10 |
| 实施例2-2 | 40％高氯酸钠混合溶液(水+10％三甘醇单甲醚)(实施例1-1) | 3 |
| 实施例2-3 | 40％高氯酸钠混合溶液(水+10％聚乙二醇200)(实施例1-2) | 3 |
| 实施例2-4 | 40％高氯酸钠混合溶液(水+10％甘油)(实施例1-3) | 3 |
| 实施例2-5 | 40％高氯酸钠混合溶液(水+20％甘油)(实施例1-4) | 3 |
| 对比例2 | 40％高氯酸钠水溶液(对比例1-1) | 3 |
根据上表2，通过加入高氯酸钠溶液，热老化性质得到明显地改善。
即使当包含水溶性有机溶剂作为水溶液的一部分时效果也完全没有损失。
工业用途的潜力
可防止含氯树脂组合物(如聚氯乙烯等)的变色和性质劣化，具体地说，其可有效地应用于所用的粘在聚氨酯泡沫体上的汽车内部装饰材料。
Claims (6)
1.用于含氯树脂稳定剂的高氯酸盐溶液，其包含1-60重量％的高氯酸盐、5-50重量％的水溶性有机溶剂、以及20-94重量％的水。
2.权利要求1的高氯酸盐溶液，其中，所述水溶性有机溶剂的沸点高于150℃。
3.用于使含氯树脂组合物热稳定的方法，特征在于，向100重量份的所述含氯树脂中加入以下物质：
(a)0.004-10重量份的高氯酸盐溶液，所述高氯酸盐溶液含有1-60重量％的高氯酸盐、5-50重量％的水溶性有机溶剂、以及20-94重量％的水；和
(b)0.001-10重量份的至少一种由以下通式(I)表示的硅酸盐化合物，
M(O)a nSiO2mH2O (I)
在通式(I)中，M是至少一种选自碱土金属和铝的金属，当M为碱土金属时a为1，当M为铝时a为3/2，n是1-5，且m是任意正整数。
4.权利要求3的方法，其中，向所述含氯树脂组合物中进一步加入0.05-10重量份的作为组分(c)的水滑石。
5.权利要求3或4的方法，其中，所述水溶性有机溶剂的沸点高于150℃。
6.含有1-60重量％的高氯酸盐、5-50重量％的水溶性有机溶剂和20-94重量％的水的高氯酸盐溶液作为用于使含氯树脂组合物热稳定的稳定剂助剂的用途。
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| PCT/JP2010/058686 WO2010131782A1 (en) | 2009-05-15 | 2010-05-17 | A perchlorate solution improved in safety, and a method for heat-stabilizing chlorine-containing resin compositions |
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| CN105295271A (zh) * | 2014-06-11 | 2016-02-03 | 中国石油化工股份有限公司 | 一种耐热高透明cpvc组合物 |
| CN115746396A (zh) * | 2022-06-27 | 2023-03-07 | 加通汽车内饰(常熟)有限公司 | 一种高氯酸盐改性水滑石及制备方法、复合热稳定剂及制备方法、皮革制品 |
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| US9205163B2 (en) | 2012-11-27 | 2015-12-08 | S.C. Johnson & Son, Inc. | Volatile material dispenser |
| WO2018039172A1 (en) | 2016-08-26 | 2018-03-01 | Galata Chemicals Llc | Heat stabilizer for halogen-containing polymers |
| JP7167535B2 (ja) * | 2018-08-07 | 2022-11-09 | 堺化学工業株式会社 | 塩素含有樹脂組成物及びその成形体 |
| CN114605758A (zh) * | 2022-04-24 | 2022-06-10 | 苏州华苏塑料有限公司 | 用于地暖地板的pvc耐磨层及其制备方法、地暖地板 |
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| CN105295271A (zh) * | 2014-06-11 | 2016-02-03 | 中国石油化工股份有限公司 | 一种耐热高透明cpvc组合物 |
| CN105295271B (zh) * | 2014-06-11 | 2017-08-25 | 中国石油化工股份有限公司 | 一种耐热高透明cpvc组合物 |
| CN115746396A (zh) * | 2022-06-27 | 2023-03-07 | 加通汽车内饰(常熟)有限公司 | 一种高氯酸盐改性水滑石及制备方法、复合热稳定剂及制备方法、皮革制品 |
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| EP2429940A1 (en) | 2012-03-21 |
| WO2010131782A1 (en) | 2010-11-18 |
| MX2011012189A (es) | 2012-01-30 |
| US20120123038A1 (en) | 2012-05-17 |
| CA2761892A1 (en) | 2010-11-18 |
| JP2012526860A (ja) | 2012-11-01 |
| BRPI1013096A2 (pt) | 2016-04-05 |
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