CN102070888B - 一种高强度聚芳醚酯组合物及其制备方法 - Google Patents
一种高强度聚芳醚酯组合物及其制备方法 Download PDFInfo
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- CN102070888B CN102070888B CN2010106149331A CN201010614933A CN102070888B CN 102070888 B CN102070888 B CN 102070888B CN 2010106149331 A CN2010106149331 A CN 2010106149331A CN 201010614933 A CN201010614933 A CN 201010614933A CN 102070888 B CN102070888 B CN 102070888B
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- 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
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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
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
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- B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
- B29C48/40—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
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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
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
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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
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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
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- B29C2948/92—Measuring, controlling or regulating
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Abstract
本发明涉及一种高强度聚芳醚酯组合物及其制备方法。该组合物，由10-60%聚芳醚酯，10-60%填充增强剂，0.3-15%液晶高分子，0.1-8.0%环氧树脂和0.1-7.0%其它助剂组成。制备方法包括如下步骤：将各组分通过双螺杆挤出机，在200-300℃的温度混合；其中，所述的液晶高分子和其它助剂中的成核剂采用侧喂失重计量的方式添加，填充增强剂采用侧喂失重方式添加；以线料排出，冷却造粒。相对于现有技术本发明在兼顾较低模温的情况下，大幅度提升了材料的强度，且具备制备工艺简单，原料成本低，产品外观优美等优点，具有良好的市场前景。
Description
技术领域
本发明涉及改性聚醚酯，具体涉及一种高强度聚芳醚酯组合物及其制备方法。
背景技术
芳香族聚醚酯，如聚对苯二甲酸乙二醇酯（PET）、聚对苯二甲酸丙二醇酯(PTT)、聚对苯二甲酸丁二醇酯(PBT)等是半结晶性热塑性树脂，具有较好的抗溶解性、高耐热性、较好的延展性、较高强度和模量，被广泛用于电子通讯设备、家电和汽车等工业制造领域。
根据不同加工或用途需要，改性芳香族聚芳醚酯已经有广泛的工业化生产。例如：
CN 01819248.3 专利公开了一种增加聚酯结晶速率的方法。该方法在聚酯内掺入有效量的超官能团成核剂，形成使聚酯结晶的稳定核。目的在于增强聚酯的透明度和耐热性。
CN03142021.4专利公开了一种化学成核玻璃纤维增强聚酯复合材料的制备方法。其特点在于，由聚合物与无机金属盐所形成的络合物作为玻璃纤维增强聚酯结晶成核剂，本发明的优点是该复合材料可在70～100℃条件下进行成型。
CN03128440.X专利涉及一种聚酯组合物。该聚酯聚合物含有热塑性聚酯、一抗冲击改性剂和聚对苯二甲酸亚丁基酯均聚物和共聚物的聚酯结晶速度增强组分。该聚酯组合物表现出增加的结晶速度。特别适合于通过热成型方法制成容器或类似的成型制品。
US363927专利则提出使用不饱和烯烃和不饱和羧酸的共聚物,如乙烯-甲基丙烯酸的共聚物,其中所有的羧酸官能团被中和从而形成碱金属盐的共聚物,作为结晶成核剂.这种结晶成核剂对于聚芳醚酯具有较好的结晶成核作用。使用这种结晶成核剂的聚芳醚酯，成型时的模温可以降低至90度左右。
上述改性方法，都是通过加快结晶速度以得到透明度、耐热性及较低模温的改性材料。由于上述方法添加增塑剂类物质，导致了产品强度偏低等缺陷。因此没能满足工业领域中对于高强度材料的需求。
发明内容
为克服以上技术缺陷，本发明采用液晶高分子为成型加工剂，采用环氧树脂为界面增强剂，提供了一种高强度聚芳醚酯组合物，并公开其制备方法。
本发明通过如下技术方案实现：
本发明涉及的高强度聚芳醚酯组合物，由10-60%聚芳醚酯，10-60%填充增强剂，0.3-15%液晶高分子，0.1-8.0%环氧树脂和0.1-7.0%其它助剂组成。
所述的聚芳醚酯为聚对苯二甲酸乙二醇酯、聚对苯二甲酸丙二醇酯或两者混合物。
所述的聚对苯二甲酸乙二醇酯优选相对密度为1.30-1.45，熔体粘度为0.5-1.0。其中，粘度的测试条件为：采用四氯乙烷和苯酚的共混溶液（重量比为40/60），在25℃下测定。理想的聚对苯二甲酸乙二醇酯是从脂肪族二羟基化合物乙二醇和芳香族二羧酸对苯二甲酸衍生的，至多10%摩尔的芳族二羧酸被间苯二甲酸或2，6-萘二酸或它们的混合物所取代；或被脂肪族或脂环族或脂环族二羧酸所取代，如己二酸、壬二酸或环己烷二羧酸等。在聚对苯二甲酸乙二醇酯中的乙二醇，基于所用的聚对苯二甲酸乙二醇酯总重量计，至多1%被1，6-己二醇和/或5-甲基-1，5-戊二醇所替代。
所述的聚对苯二甲酸丙二醇酯（PTT），优选的相对密度为1.28-1.38，熔体粘度为0.5-1.0。粘度的测试条件为：采用四氯乙烷和苯酚的共混溶液（重量比为60/40），在25℃下测定。理想的聚对苯二甲酸丙二醇酯是从脂肪族二羟基化合物丙二醇和芳香族二羧酸对苯二甲酸衍生的，至多10%摩尔的芳族二羧酸被间苯二甲酸或2，6-萘二酸或它们的混合物取代；或被脂肪族或脂环族或脂环族二羧酸所取代，如己二酸、壬二酸或环己烷二羧酸等。在聚对苯二甲酸乙二醇酯中的乙二醇也可以被至多1%重量的物质替代，如被1，6-己二醇和/或5-甲基-1，5-戊二醇所替代，基于所用的聚对苯二甲酸乙二醇酯总重量计。
所述的填充增强剂优选云母粉、高岭土、硅灰石、玻璃粉、玻璃微珠、玻璃片、蒙脱土、硫酸钡、玻璃纤维、矿物纤维、碳纤维等一种或几种的混合物。矿物纤维和玻璃纤维优选为直径为5-15um的短切纤维，更优选为7-13um的短切纤维，最优选为7-10um的短切纤维。
本发明所采用液晶高分子（LCP）是热致型液晶高分子，在270度-360度间可以形成各向异性的树脂，优选为在280-330度可以形成各向异性的树脂。其中所述的液晶高分子（LCP）为的链结构中包含了由p-对羟基苯甲酸(HBA)、对苯二酚(HQ)、混合芳香二酸(MA,由间苯二甲酸(IA)、2,6-萘二酸(NDA)、4,4’-二羧基-N-苯基苯甲酰胺(NA)混合而成)、对苯二甲酸(TA)、4,4’-二苯醚二甲酸(DODA)引出的一种或多种重复单元。
所述的环氧树脂可由多元酚与多元醇与环氧氯丙烷经缩聚反应而制得。环氧树脂包括：双酚 A-二缩水甘油醚、双酚F二缩水甘油醚、脂肪醇多缩水甘油醚、线形酚醛多缩水甘油醚、缩水甘油酯型环氧树脂、缩水甘油胺型环氧树脂、脂环族环氧树脂、线形脂肪族环氧树脂。环氧树脂优选为二氧化二聚环戊二烯类环氧树脂，如
二氧化乙烯基环己烯
3,4-环氧基环己甲酸-3′，4′-环氧基环己甲酯
二氧化双环戊二烯
3,4-环氧基-6-甲基环己甲酸-3′，4′-环氧基-6-甲基环己甲酯 
二氧化二戊烯 
二氧化双环戊基醚
所述的其他助剂包括抗氧剂、脱模剂、热稳定剂、颜料、UV稳定剂、润滑剂、成核剂、增韧剂、界面改性剂、扩链剂。
所述的抗氧剂包括四[β-（3,5-二叔丁基-4-羟基苯基）丙酸]季戊四醇酯（Irganox 1010）、1,3,5-三甲基-2,4,6-三（4`-羟基-3`,5`-二叔丁基苄基）苯（Irganox 1330）、己二醇[β-(3,5-二叔丁基-4-羟基苯基)丙酸酯（Irganox 259）、2,2`-亚硫基乙二醇双[β-(3,5-二叔丁基-4-羟基苯基)丙酸酯](如Irganox 1035)、N,N`-六亚甲基双（3,5-二叔丁基-4-羟基苯丙酰胺）（Irganxo 1098）、亚磷酸三（2,4-二叔丁基苯基）酯（如Irgafos 168）、双（2,4-二叔丁基苯基）季戊四醇二亚磷酸酯（如Ultranox 626GE）或硫代二丙酸二月桂酯（Nonox DLTP）；四(2,4-二叔丁基酚)-4,4'-联苯基二亚磷酸酯（IRGAFOS P-EPQ）、双(2,6-二叔丁基-4-甲基苯基)季戊四醇二磷酸酯（ADK Stab PEP-36）。其中，所述的抗氧剂优选为1010和P-EPQ。
其中，所述的界面改性剂优选为 γ- 氯丙基三甲氧基硅烷、γ-氨丙基三乙氧基硅烷, 聚乙烯吡咯烷酮、γ-氨丙基甲基二乙氧基硅烷、钛酸四正丙酯、聚钛酸丁酯、 四正丙基锆酸酯 , 四（三乙醇胺）锆酸酯、二硬脂酰氧异丙氧基铝酸酯、γ-（2，3-环氧丙氧）丙基三甲氧基硅烷 。
其中所述的增韧剂包括马来酸酐或环氧基团官能化的橡胶类共聚物、烯烃和丙烯酸酯类共聚物，例如乙烯-丙烯酸乙酯-甲基丙烯酸缩水甘油酯三聚物、乙烯-丙烯酸丁酯-甲基丙烯酸缩水甘油酯三聚物、乙烯-醋酸乙烯共聚物-功能化马来酸酐、苯乙烯-乙烯丁烯-苯乙烯-功能化马来酸酐、乙烯-丙烯酸甲酯共聚物、乙烯-丙烯酸乙酯共聚物、乙烯-丙烯酸丁酯共聚物、甲基丙烯酸甲酯-丁二烯-苯乙烯接枝共聚物。
其中所述的扩链剂包括二异氰酸酯、二酐或二恶唑啉类物质，例如，均苯四酸二酐、偏苯三酸酐、苯并双恶唑、羰基双（1-己内酰胺）、亚磷酸三苯酯、四环氧四缩水甘油二氨基二苯甲烷等。
其中，所述的颜料优选二氧化钛、硫化锌、立德粉、炭黑或有机色粉。
其中，所述的UV稳定剂优选为苯并唑衍生物。
其中，所述的脱模剂优选为脂肪酸酯。
其中，所述的成核剂优选为有机钠化合物，如脂肪酸钠盐、脂肪酸锌盐或脂肪酸钙盐、褐煤酸钠、苯甲酸钠、氯苯甲酸钠、乙烯-丙烯酸钠离子聚合物、乙烯-甲基丙烯酸钠离子聚合物以及页硅酸盐类粘土化合物，如滑石粉、云母、高岭土等。
所述的组合物的制备方法，其特征在于包括如下步骤：各组分通过双螺杆挤出机，在200-300℃的温度混合；其中，所述的液晶高分子和其它助剂中的成核剂采用侧喂失重计量的方式添加，填充增强剂采用侧喂失重方式添加；以线料排出，冷却造粒。
相对于现有技术，本发明采用液晶高分子为成型加工剂，采用环氧树脂为界面增强剂，由于不含有增塑剂，原料对苯二甲酸乙二醇酯等芳香族聚醚酯组合物被优选注射到模具中，该模具应该保持较高的温度，以获得具有高结晶度和优异尺寸稳定性的模塑部件。由于实用方面的考量，较低的模具温度是合适的。因此，在本发明中，优选的模具温度在90-150度、更优选在100-140度、最优选在115-130度，这里的温度单位是摄氏度。
本发明涉及的聚芳醚酯组合物在兼顾较低模温的情况下，大幅度提升了材料的强度，且具备制备工艺简单，原料成本低，产品外观美等优点，具有良好的市场前景。
具体实施方式
按不同组分，设计8个实施例，具体组分如下A、B、C、D、E所示，具体配比见表1和表2。
A：两种PET树脂作为范例，特性粘度分别为A1:[η]A1=0.58dl/g，A2: [η]A2=0.83 dl/g，采用四氯乙烷/苯酚（4：6）为溶液，在25度下测定；A3:一种PTT树脂作为范例，特性粘度为[η]A3=0.71dl/g，，采用四氯乙烷/苯酚（6：4）为溶液，在25度下测定。
B：玻璃纤维（ECS303A（E），重庆国际复合材料有限公司）
C：LCP
D：环氧树脂，Unox Ep201 3,4-环氧基-6-甲基环己甲酸-3′，4′-环氧基-6-甲基环己甲酯
E：其他助剂
制备方法：将各组分在双螺杆挤出机（双螺杆直径为75mm，长径比为38），在200-300℃的温度混合，其中成核剂和LCP采用侧喂失重计量的方式添加，而填充增强剂采用另一个侧喂失重方式添加，以线料排出并在冷却至能够造粒的温度后造粒。粒料干燥（通常在80℃、真空干燥箱中持续2日）后，将所得干燥后粒料在245℃-290℃的温度下加工成根据GB1040，GB9341，GB1843规定的标准样条，其中模具温度为120度。
通过强度实验测试，结果如表1和表2所示。
表1
| 实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 | 实施例6 | ||
| A1 | % | 63 | 60 | 55 | |||
| A2 | 63 | 60 | 65 | ||||
| B | % | 30 | 30 | 30 | 30 | 30 | 30 |
| C | % | 2 | 5 | 10 | 2 | 5 | |
| D | % | 1 | 1.2 | 1 | 1.2 | ||
| E | % | 5 | 4 | 3.8 | 5 | 4 | 3.8 |
| 拉伸强度 | Mpa | 139 | 165 | 185 | 155 | 162 | 141 |
| 弯曲强度 | Mpa | 213 | 241 | 258 | 233 | 238 | 211 |
表2
| 实施例7 | 实施例8 | ||
| A3 | % | 60 | 55 |
| B | % | 30 | 30 |
| C | % | 5 | 10 |
| D | % | 1.5 | |
| E | % | 5 | 3.5 |
| 拉伸强度 | Mpa | 132 | 165 |
| 弯曲强度 | Mpa | 205 | 238 |
从以上两表格的数据可以看出，含有液晶高分子为成型加工剂和采用环氧树脂为界面增强剂的实施例的强度明显优于不含以上组分的组合物。
Claims (7)
1.一种高强度聚芳醚酯组合物，该组合物由如下重量配比的组分组成：聚芳醚酯 55-60%，填充增强剂 10-60%，液晶高分子 0.3-15%，环氧树脂 1-1.5%，其他助剂 0.1-7.0%，其中各组分的重量百分比之和为100%；其中所述的聚芳醚酯为聚对苯二甲酸乙二醇酯或聚对苯二甲酸丙二醇酯；所述的环氧树脂是脂环族环氧树脂。
2.根据权利要求1所述的组合物，其特征在于，所述的填充增强剂为云母粉、高岭土、硅灰石、玻璃粉、玻璃微珠、玻璃片、蒙脱土、硫酸钡、玻璃纤维、矿物纤维或碳纤维中的一种或几种的混合物。
3.根据权利要求2所述的组合物，其特征在，所述的矿物纤维或玻璃纤维的直径为5-15μm的短切纤维。
4.根据权利要求1所述的组合物，其特征在于，所述的液晶高分子为在270度-360度间能形成各向异性的热致型液晶高分子树脂。
5.根据权利要求1所述的组合物，其特征在于，所述的其他助剂为抗氧剂、脱模剂、热稳定剂、颜料、UV稳定剂、润滑剂、成核剂、增韧剂、界面改性剂或扩链剂中的一种或几种的混合物。
6.根据权利要求5所述的组合物，其特征在于，所述界面改性剂选自 γ- 氯丙基三甲氧基硅烷、γ-氨丙基三乙氧基硅烷、 聚乙烯吡咯烷酮、γ-氨丙基甲基二乙氧基硅烷、钛酸四正丙酯、聚钛酸丁酯、 四正丙基锆酸酯 、四（三乙醇胺）锆酸酯、二硬脂酰氧异丙氧基铝酸酯或γ-（2，3-环氧丙氧）丙基三甲氧基硅烷中的一种或者几种。
7.权利要求1到6任一权利要求所述的组合物的制备方法，其特征在于包括如下步骤：各组分通过双螺杆挤出机，在200-300℃的温度混合；其中，所述的液晶高分子和其他助剂中的成核剂采用侧喂失重计量的方式添加，填充增强剂采用侧喂失重方式添加；以线料排出，冷却造粒。
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