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CN1137026C - 连续制备氨基塑料和/或酚醛塑料的方法 - Google Patents

连续制备氨基塑料和/或酚醛塑料的方法 Download PDF

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CN1137026C
CN1137026C CNB988083027A CN98808302A CN1137026C CN 1137026 C CN1137026 C CN 1137026C CN B988083027 A CNB988083027 A CN B988083027A CN 98808302 A CN98808302 A CN 98808302A CN 1137026 C CN1137026 C CN 1137026C
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H·贝尔布纳
H·埃特林
E·古恩特
T·西尔克
H·D·策特勒
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Abstract

本发明涉及连续制备氨基塑料和/或酚醛树脂的方法；其中，预缩合物溶液在第一挤压机(14)中制备，预缩合物溶液，与添加剂的加入一起，连续喂入在进料段(E)和脱挥发物段(G)中有局部填充的第二个挤压机(20)；其在第二个挤压机(20)中脱挥发物，然后使其成形为模塑组合物或最后产物。该方法特别适于制备密胺树脂，特别是密胺-甲醛树脂，以及特别适于制备尿素-甲醛树脂。

Description

连续制备氨基塑料和/或酚醛塑料的方法
本发明是关于制备氨基塑料及/或酚醛塑料的方法，以及制备密胺树脂及/或酚醛树脂，尤其是密胺-甲醛树脂、尿素-甲醛树脂、酚醛树脂及其掺合物的方法。
氨基塑料(直接抑或于半成品的进一步成形期间硬化的注塑或压塑制品)有良好的机械性质、高火焰阻滞性、耐热性和抗溶剂性、高耐刮伤性及良好的外观(表面)。与聚酰胺或其它工程塑料比较，制备氨基塑料的原材料的价格较便宜。
制备密胺树脂半成品或成品零件的已用方法有下列一系列步骤：先在可加热混合容器中，将原材料分批预缩合，以给与具有约50％浓度的胺-甲醛树脂溶液，将所产生的溶液喷雾干燥，以给与密胺-甲醛树脂粉末，在下一步骤中于，例如，犁型混合器中，使所产生的树脂粉末与填料一起干式混合，接着借助可加热砑光机连续塑化，以给与配混料，然后在下一步骤中，先粗粉碎，接着细碾磨；将各批混合以给与均匀的颜色并将材料再次压紧以给与自由流动的模塑组合物，及最后注射模塑或压缩塑制成成品零件。
在“单程”反应器中制备密胺-甲醛树脂的简化方法说明于US4,458,062。此处重要的是原材料为结晶密胺和固态甲醛，并且操作是在没有水或任何其它溶剂存在的情形下进行。然而，固态甲醛比液态甲醛溶液昂贵。另外，此方法所给与的密胺-甲醛树脂的性质明显地不同于有溶剂存在下所制备的树脂的性质。
DE-A 24 51 874说明一种制备氨基塑料的改良方法，其中预缩合物水溶液(若须要可与颜料的添加一起)进入流化床干燥器并喷在填料上，干燥，然后接着切粒并直接作为模塑组合物使用。
本发明的主旨是提供一种连续性方法，其使得以少数步骤制备氨基塑料的简单且低成本的方法成为可能。此外，此新方法应使得氨基塑料的加工和产品性质，可在广泛的范围内，以简单的方法，逐一地调整。
已发现，此主旨是借助下面的方法完成，其中预缩合物溶液是在第一个挤压机中制备，预缩合物溶液，在加入添加剂的情况下，连续馈入在进料段(E)和脱挥发物段(G)中有局部填充物的第二个挤压机，该溶液于第二个挤压机内脱挥发物，然后接着成形以给与最后产物。
已发现，于第二个挤压机内，适当选定的添加剂的加添，使得调整树脂的反应性或进行产物性质(例如，尤其是冲击强度或其它机械性质)方面的控制性改良是可行的。此外，本方法使产物的残余湿气可在第二个挤压机内，借助脱挥发物系统来调节。
在本新方法中，预缩合物溶液是以从EP-B 0 355 760中所知的方法先制备，该方法是使原材料(例如，密胺及甲醛水溶液)与(若须要)多聚甲醛，以密胺：甲醛的摩尔比为1∶1.5至1∶3，较佳是1∶2至1∶3的比例混合，若须要可加入不干扰缩合反应的已知改良剂和添加剂，例如，一元醇、二元醇、磺胺、糖、碱性催化剂(例如，胺、氨基醇和羟基烷基密胺)，然后使其在第一个挤压机中，以120至140℃预缩合至相当于粘度上升至至少1Pa.s的缩合度。预缩合物溶液有60至90％的固体含量，较佳是75至80％。
尿素-甲醛预缩合物溶液可由尿素溶液和甲醛溶液(若须要，可带有适当添加剂)以相应方法制备。
方法的重要单元为第二个挤压机，喂入其中的是在第一个挤压机中以已知的方法制备的预缩合物溶液。虽然第一个挤压机必须100％充满，以致于停留时间可准确调节，以给与限定的缩合度，但根据本发明，第二个挤压机必须于进料段(E)和脱挥发物段(G)中是局部充满。这不仅使得先将添加剂直接加至第二个挤压机中成为可能，该添加剂可用于调整氨基塑料的加工和产物性质，而且接着在第二个挤压机中进行物质的脱挥发作用，由于所产生的固体的排放，所以脱挥发作用将不可能在完全充满的挤压机内进行。
第一个挤压机最好是以每分钟约12至20转的旋转速率操作，而第二个挤压机最好是每分钟20至300转，特别好地是每分钟80至150转。
第二个挤压机的温度可借助温度传感器(温度指示控制器(TIC))分区控制，设定值有利地是30至170℃，较佳是80至120℃。
在第二个挤压机的末端，加入使产物的接着的固化作用发生的酸式催化剂。
连接于第二个挤压机的是，以适合的方法使最后产物的成形发生的设备：
在第一种方法中，于第二个挤压机中脱挥发物的完全配制好的模塑组合物可经多股膜头挤出、切粒、给与最后的干燥作用并冷却。粒料具有与商业供应的模塑组合物类似的性质并可借助，例如，注射模塑进一步加工。
在第二种方法中，在挤压机的末端可使用挤片模头，并且经此模头，可使原料模塑组合物成形为连续薄片。要在此调整工艺参数，以使薄片有充分的尺寸稳定性，但尚未完全固化。接着，将所制得的薄片定型和冷却。如此给予适于销售的产物，其是能再加工的半成品，并且其可在可加热压机上再成形，以给予想要的固化的成品零件。
在第三种方法中，将连续薄片定型，并借助连接在挤片模头的下游处的可加热带式压机而以130至190℃完全固化。完全固化的模塑制品可在多种应用领域中使用，尤其是用在电子、建筑和汽车等领域。
使用后文的图示和操作实例进一步举例说明本发明。
本发明附图1为本发明方法的示意图。
来自储槽3的密胺和来自储槽1的多聚甲醛是借助连续称重给料器5和6喂入混合器11中。来自搅拌储槽2的液态甲醛溶液，来自槽9的二乙基乙醇胺和来自槽4的含水5-羟基-3-氧杂戊基密胺混合物，借助计量泵7、8和10，亦喂入混合器11内。悬浮液于槽12内脱挥发物，然后借助泵13，计量进入第一个可加热连续挤压机14。此后，固态组份溶解并产生树脂似的预缩合物16。将预缩合物形成为约80％浓度的高粘性水溶液。
预缩合液16是直接亦或借助计量泵15喂入第二个挤压机20。来自储槽17的干式混合过的添加剂，借助重量计量系统18，亦喂入第二个挤压机20。于第二个挤压机20的末端处的挤片模头21连续地使模塑组合物成形以给与原料薄片。
实施例
预缩合物溶液是在第一个挤压机14中，按照表1所示配方，以由EP-B 0 355 760中所知的方法来制备。
            表1：预缩合物溶液的配方
重量％ 摩尔％，以∑三嗪为基准
∑三嗪，其中密胺5-羟基-3-氧杂戊基密胺混合物 43.3515.69 1009010
双酚A 1.14 1.3
∑甲醛，其中多聚甲醛甲醛(40％) 11.7228.10 200
二乙基乙醇胺 0.17 0.4
可能的添加剂为可改变加工及/或产物性质的那些，例如，纤维状或粉状无机增强剂或填料，像玻璃纤维、金属粉末、金属盐类或硅酸盐，生物性增强剂或填料，像纤维素纤维、纸浆或木粉；增弹剂，像丙烯酸酯，橡胶，聚乙二醇；二醇，山梨糖醇，糖，颜料，UV稳定定剂；反应阻滞剂，像胺；润滑剂，缓冲剂或不粘结剂。
表2给出具有下列添加剂的模塑组合物配方的实例：作为填料的纤维素，作为改性剂的二乙二醇(特别为了增进抗龟裂性)，作为润滑剂的硬脂酸盐混合物，作为缓冲剂的碳酸钠和作为不粘结剂的邻苯二甲酸二烯丙酯。
            表2：模塑组合物配方
   重量％
依表1配制的80％预缩合物溶液    60.91
添加剂    ∑39.09
纤维素(填料)    30.46
二乙二醇(阻滞剂，增塑剂)    4.06
硬脂酸盐混合物(润滑剂)    2.73
苏打(缓冲剂)    0.91
邻苯二甲酸二烯丙酯(不粘结剂)    0.91
第二个挤压机20内的温度最好是借助温度传感器(TIC)来控制，设定值有利地是30至170℃，较佳是80至120℃。
在第二个挤压机20中，反应混合物是借助真空泵来脱挥发物，如此使得将模塑组合物的残余湿气调整至较佳的8至15％范围内是可能的。于第二个挤压机20的末端处的挤片模头21连续地使模塑组合物成形以给与原料薄片，其在阳模内以140℃固化0.5至10分钟，较佳是1至3分钟。
测试已成形且固化的薄片的挠曲强度和冲击强度。为对照，由瑞清(Raschig)商业供应的密胺-甲醛模塑组合物MF 152，在阳模内以140℃固化不超过5分钟，并测量其机械性质。达到DIN 7708-152 N的材料品质标准。
            表3：机械性质
根据DIN53452的挠曲强度N/mm2，(23℃) 根据ISO 179的冲击强度k.J/m2，(23℃)
来自操作实例的模塑制品 102 6.6
来自瑞清(Raschig)模塑组合物MR 152的模塑制品 76 4.8

Claims (18)

1.一种制备氨基塑料和/或酚醛塑料的方法，其中预缩合物溶液是在第一个挤压机中制备，其包括将预缩合物溶液(16)在添加添加剂的情况下连续喂入在进料段(E)和脱挥发物段(G)中有局部填充的第二个挤压机(20)，于第二个挤压机(20)内将预缩合物溶液脱挥发物，然后使其成形以获得最后产物。
2.根据权利要求1的方法，其中第一个挤压机是以12至20分钟-1的旋转速率操作，而第二个挤压机是以20至300分钟-1的旋转速率操作。
3.根据权利要求2的方法，其中第一个挤压机是以12至20分钟的旋转速率操作，而第二个挤压机是以80至150分钟-1的旋转速率操作。
4.根据权利要求1的方法，其中第二个挤压机(20)要在30至170℃下加热。
5.根据权利要求2的方法，其中第二个挤压机(20)要在30至170℃下加热。
6.根据权利要求3的方法，其中第二个挤压机(20)要在30至170℃下加热。
7.根据权利要求4-6中任何一项的方法，其中第二个挤压机(20)要在80至120℃下加热。
8.根据权利要求1-6中任何一项的方法，其中残余湿分是在第二个挤压机内调整至8至15重量％水。
9.根据权利要求7的方法，其中残余湿分是在第二个挤压机内调整至8至15重量％水。
10.根据权利要求1-6中任何一项的方法，其中最后产物为模塑组合物。
11.根据权利要求7的方法，其中最后产物为模塑组合物。
12.根据权利要求1-6中任何一项的方法，其中最后产物为能够进一步成形的半成品。
13.根据权利要求7的方法，其中最后产物为能够进一步成形的半成品。
14.根据权利要求1-6中任何一项的方法，其中最后产物为成品零件。
15.根据权利要求7的方法，其中最后产物为成品零件。
16.根据权利要求1-15中任何一项的方法制备密胺树脂的应用。
17.根据权利要求1-15中任何一项的方法制备密胺-甲醛树脂的应用。
18.根据权利要求1-15中任何一项的方法制备尿素-甲醛树脂的应用。
CNB988083027A 1997-08-18 1998-08-13 连续制备氨基塑料和/或酚醛塑料的方法 Expired - Fee Related CN1137026C (zh)

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