CN101134847B - 一种聚苯硫醚/聚酰胺复合材料及其制备方法 - Google Patents
一种聚苯硫醚/聚酰胺复合材料及其制备方法 Download PDFInfo
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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
- B29C48/03—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
- B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
- 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
- B29C48/88—Thermal treatment of the stream of extruded material, e.g. cooling
- B29C48/918—Thermal treatment of the stream of extruded material, e.g. cooling characterized by differential heating or cooling
- B29C48/9185—Thermal treatment of the stream of extruded material, e.g. cooling characterized by differential heating or cooling in the direction of the stream of the material
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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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- B29C48/95—Lubricating by adding lubricant to the moulding material
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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
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
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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
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
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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
- B29C2948/00—Indexing scheme relating to extrusion moulding
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- B29C2948/92819—Location or phase of control
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Abstract
本发明公开了一种聚苯硫醚/聚酰胺复合材料及其制备方法，聚苯硫醚/聚酰胺复合材料由以下配比的原料按重量百分比配制而成：聚苯硫醚(PPS)23-69.3％，聚酰胺(PA)10-30％，玻璃纤维(GF)20-40％，热稳定剂0.2-2％，硅烷偶联剂0.1-2％，加工润滑剂0.2-2％，结晶促进剂0.1-1％。本发明聚苯硫醚/聚酰胺复合材料克服聚苯硫醚冲击强度低，耐弯折性差的缺点，提高材料的冲击韧性，本发明所提出的聚苯硫醚(PPS)/聚酰胺(PA)复合材料的制备工艺简单、产品成本低廉。
Description
[技术领域]
本发明涉及聚苯硫醚树脂材料，尤其涉及一种聚苯硫醚/聚酰胺复合材料及其制备方法。
[背景技术]
聚苯硫醚树脂(PPS)也称聚亚苯基硫醚，其综合性能较好，耐高温、耐腐蚀、耐辐射、不燃、并具备良好的机械性能和电性能，因而聚苯硫醚是电子、电器领域的首选材料。但聚苯硫醚树脂(PPS)冲击强度低，耐弯折性差；而且PPS熔体黏度大，加工性能不够好；同时其成本相对于通用工程塑料成本也较高。这些缺点限制了聚苯硫醚树脂在中端产品领域的应用范围。针对聚苯硫醚树脂性能上的缺陷，国内外研究非常活跃，但至今仍没有突破性的开发成果问世。
[发明内容]
本发明要解决的技术问题是提供一种聚苯硫醚复合材料，它能够克服聚苯硫醚冲击强度低，耐弯折性差的缺点，提高材料的冲击韧性。
本发明进一步要解决的技术问题是提供一种熔体粘度低，加工流动性好的聚苯硫醚复合材料。
为了解决上述技术问题，本发明采用的技术方案是，一种聚苯硫醚/聚酰胺复合材料，它由以下配比的原料按重量百分比配制而成：
聚苯硫醚(PPS) 23-69.3％
聚酰胺(PA) 10-30％
玻璃纤维(GF) 25-35％
热稳定剂 0.2-2％
硅烷偶联剂 0.1-2％
加工润滑剂 0.2-2％
结晶促进剂 0.1-1％。
其中，所述聚酰胺树脂的相对密度为1.12-1.15g/cm3，熔点为255-265℃，熔体粘度为0.3-3；所述聚苯硫醚树脂相对密度为1.3-1.4g/cm3，分子量为40000-50000；所述结晶促进剂为一种有机成分和无机成分的细致粉末混合物；所述的热稳定剂为粉末状的无机磷酸 盐；所述的玻璃纤维的直径为6-17微米；所述的硅烷偶联剂为γ-氨丙基三乙氧基硅烷。
以上所述的聚苯硫醚/聚酰胺复合材料，它最好由以下配比的原料按重量百分比配制而成：
聚苯硫醚(PPS) 44-55％
聚酰胺(PA) 15-25％
玻璃纤维(GF) 25-35％
热稳定剂 0.2-0.4％
硅烷偶联剂 0.1-0.4％
加工润滑剂 0.2-0.4％
结晶促进剂 0.2-0.4％。
本发明的有益效果是：
1.通过在体系中添加聚酰胺树脂后，整体复合材料的韧性和抗折弯的能力大幅度提高，并且在保留了聚苯硫醚本身所具有的高耐温、尺寸稳定性好等优异特点的前提下，其耐磨性和产品外观 也得到了很大改善，具有一定自熄性，符合环保要求，应用前景广阔。
2.本发明所采用的助剂，如聚酰胺、玻璃纤维、结晶促进剂、热稳定剂、偶联剂等组分，均为价格低廉的市售产品，材料的生产成本较低；本发明所提出的聚苯硫醚(PPS)/聚酰胺(PA)复合材料的制备工艺简单、成本低。
本发明在聚苯硫醚材料中添加聚酰胺树脂及其结晶体系后，使材料熔体粘度降低，尤其当聚酰胺树脂的添加量超过15％时，熔体粘度明显降低，降低了加工温度，复合材料的加工温度范围明显变宽、加工条件的可调节性提高，更易于注塑一些复杂结构的制件。
[具体实施方式]
下面通过实施例对本发明进行进一步阐述：
本发明使用的聚酰胺树脂的相对密度为1.12-1.15g/cm3，熔点为255-265℃，熔体粘度为0.3-3；聚苯硫醚树脂相对密度为1.3-1.4g/cm3，分子量为40000-50000；结晶促进剂为一种有机成分和无机成分的细致粉末混合物；热稳定剂为三甘醇双-3-(3-叔丁基-4羟基-5-甲基苯基)丙稀腈、三(2，4-二叔丁基酚)亚磷酸酯的一种；玻璃纤维的直径为6-17微米；硅烷偶联剂为γ-氨丙基三乙氧基硅烷或γ-(2、3环氧丙氧)丙基三甲氧基硅烷。
在实施例的复合材料配方中，聚苯硫醚为支链型结构产品，密度 大约为1.3-1.4g/cm3，分子量为40000-50000，为Philips公司生产，商品牌号为Ryton PR37；聚酰胺树脂为粘度约为2.0-3.0的聚己二酰己二胺(PA66)，为Rhodia公司生产，商品牌号为27AE1B；热稳定剂为粉末状的无机磷酸盐，为Bruggemann公司生产，商品牌号为BRUGGOLEN H161；结晶促进剂为德国Clariant公司生产，商品牌号为CAV101；璃纤维直径为5-20微米；其中硅烷偶联剂KH550化学名称为γ-氨苯基三乙氧基硅烷；润滑剂为Dow Corning公司生产，商品牌号为MB-50；
实施例1
将重量比为PPS---58.9％、PA66---10％、玻璃纤维---30％、偶联剂---0.2％、CAV101---0.3％、H161---0.3％、润滑剂---0.3％干混4分钟，之后，再在双螺杆挤出机同表面经偶联剂KH550处理过的玻璃纤维30％掺混，经熔融挤出、造粒制成复合材料。其中螺杆各加温区设置分别为：一区270℃，二区280℃，三区290℃，四区300℃，停留时间为2分钟，压力为20Mpa。
实施例2
将重量比为PPS---54.9％、PA66---15％、玻璃纤维---29％、偶联剂---0.2％、CAV101---0.3％、H161---0.3％、润滑剂---0.3％干混4分钟，之后，再在双螺杆挤出机同表面经偶联剂KH550处理过的玻璃纤维29％掺混，经熔融挤出、造粒制成复合材料。其中螺杆各加温区设置分别为：一区270℃，二区280℃，三区290℃，四区300℃，停留时间为2分钟，压力为20Mpa。
实施例3
将重量比为PPS---49.9％、PA66---20％、玻璃纤维---29％、偶联剂---0.2％、CAV101---0.3％、H161---0.3％、润滑剂---0.3％干混4分钟，之后，再在双螺杆挤出机同表面经偶联剂KH550处理过的玻璃纤维29％掺混，经熔融挤出、造粒制成复合材料。其中螺杆各加温区设置分别为：一区270℃，二区280℃，三区290℃，四区300℃，，停留时间为2分钟，压力为20Mpa。
实施例4
将重量比为PPS---44.9％、PA66---25％、玻璃纤维---29％、偶联剂---0.2％、CAV101---0.3％、H161---0.3％、润滑剂---0.3％干混4分钟，之后，再在双螺杆挤出机同表面经偶联剂KH550处理过的玻璃纤维29％掺混，经熔融挤出、造粒制成复合材料。其中螺杆各加温区设置分别为：一区270℃，二区280℃，三区290℃，四区300℃，，停留时间为2分钟，压力为20Mpa。
实施例5
将重量比为PPS---39.9％、PA66---30％、玻璃纤维---29％、偶联剂---0.2％、CAV101---0.3％、H161---0.3％、润滑剂---0.3％干混4分钟，之后，再在双螺杆挤出机同表面经偶联剂KH550处理过的玻璃纤维29％掺混，经熔融挤出、造粒制成复合材料。其中螺杆各加温区设置分别为：一区270℃，二区280℃，三区290℃，四区300℃，，停留时间为2分钟，压力为20Mpa。
对比例
将重量比为PPS---69.9％、玻璃纤维---29％、偶联剂---0.2％、H161---0.3％、润滑剂---0.3％干混4分钟，之后，再在双螺杆挤出机同表面经偶联剂KH550处理过的玻璃纤维29％掺混，经熔融挤出、造粒制成复合材料。其中螺杆各加温区设置分别为：一区270℃，二区280℃，三区290℃，四区300℃，停留时间为2分钟，压力为20Mpa。
性能评价方式及实行标准：
将按上述方法完成造粒的粒子材料预先在100℃的鼓风烘箱中干燥3-6小时，然后再将干燥好的粒子材料在注射成形机上进行注射成型制样，注射成型模温控制在120℃左右。
拉伸强度测试按ISO527-2进行，试样尺寸为150×10×4mm，拉伸速度为50mm/min；弯曲性能测试按ISO 178进行，试样尺寸为80×10×4，弯曲速度为2mm/min，跨距为64mm；简支梁冲击强度按ISO 179进行，试样尺寸为55×6×4mm，缺口尺寸为试样厚度的三分之一；热变形温度测试按ISO 75-2进行测试，试样尺寸为150×15×10mm，最大变形量为0.32mm；
综合力学性能通过测试所得的拉伸强度、断裂伸长率、弯曲模量以及冲击强度的数值进行评判；
实施例1-5以及对比例1-2的配方及力学性能测试结果见表1及表2；
表1实施例及对比例的配方及材料性能表
| 组成 | 实施例1 | 实施例2 | 实施例3 |
| PPS(％) | 58.9 | 54.9 | 49.9 |
| PA66(％) | 10 | 15 | 20 |
| GF(％) | 30 | 29 | 29 |
| CAV101(％) | 0.3 | 0.3 | 0.3 |
| H161(％) | 0.3 | 0.3 | 0.3 |
| KH550(％) | 0.2 | 0.2 | 0.2 |
| MB-50(％) | 0.3 | 0.3 | 0.3 |
| 缺口冲击 强度(KJ/M2) | 16 | 17.6 | 19 |
| 拉伸强度 (Mpa) | 165 | 162 | 156 |
| 断裂伸长 率(％) | 2 | 3.5 | 4.5 |
| 弯曲强度 (Mpa) | 225 | 220 | 215 |
| 弯曲模量 (Mpa) | 10800 | 10300 | 9900 |
| 热变形温 度(℃) | 265 | 263 | 260 |
表1续
| 组成 | 实施例4 | 实施例5 | 对比例2 |
| PPS(％) | 44.9 | 39.9 | 69.9 |
| PA66(％) | 25 | 30 | / |
| GF(％) | 29 | 29 | 30 |
| CAV101(％) | 0.3 | 0.3 | 0.3 |
| H161(％) | 0.3 | 0.3 | 0.3 |
| KH550(％) | 0.2 | 0.2 | 0.2 |
| MB-50(％) | 0.3 | 0.3 | 0.3 |
| 缺口冲击 强度(KJ/M2) | 20.8 | 21.5 | 13 |
| 拉伸强度 (Mpa) | 150 | 150 | 165 |
| 断裂伸长 率(％) | 5 | 6.5 | 2 |
| 弯曲强度 (Mpa) | 210 | 205 | 225 |
| 弯曲模量 (Mpa) | 9600 | 5 | 10800 |
| 热变形温 度(℃) | 248 | 245 | 265 |
通过表1实施例1-5同对比例的各项性能分析可知，聚苯硫醚(PPS)/聚酰胺(PA)复合材料的综合力学性能较好，而且对比单纯PPS增强材料，其机械性能和热性能下降幅度较小。并且从表1实施例1-5的各项性能数据来看，在添加了尼龙树脂进入PPS体系中以后，整体复合材料的韧性得到了大幅度提升，除实施例1外熔体粘度也下降明显，而且结晶促进剂的加入也加速了整体复合材料的结晶速度，所形成的晶粒细小均匀，使得整体材料的强度高。但尼龙树脂添加量过多会影响材料的综合物理力学性能，导致材料的机械性能和热性能下降较大，从而丧失了PPS作为特种工程塑料的使用价值。PA66添加量为20％，CAV101含量为0.3％，热稳定剂为0.3％时材料的综合力学性能、热性能以及性价比均较好，经过以上改性处理的复合材料综合性能优异。
本发明的聚苯硫醚(PPS)/聚酰胺(PA)复合材料，其具有制备工艺简单、成本适中、各项物理化学性能优异、耐热性能接近单纯PPS增强材料等特点，可用于电子、电器元件、汽车配件以及机械电子领域等技术领域。
Claims (8)
1.一种聚苯硫醚/聚酰胺复合材料，其特征在于，它由以下配比的原料按重量百分比配制而成：
聚苯硫醚(PPS) 23-69.3％
聚酰胺(PA) 10-30％
玻璃纤维(GF) 25-35％
热稳定剂 0.2-2％
硅烷偶联剂 0.1-2％
加工润滑剂 0.2-2％
结晶促进剂 0.1-1％。
2.根据权利要求1所述的聚苯硫醚/聚酰胺复合材料，其特征在于：
所述聚苯硫醚树脂相对密度为1.3-1.4g/cm3，分子量为40000-50000。
3.根据权利要求1所述的聚苯硫醚/聚酰胺复合材料，其特征在于：
所述聚酰胺树脂的相对密度为1.12-1.15g/cm3，熔点为255-265℃，熔体粘度为0.3-3。
4.根据权利要求1所述的聚苯硫醚/聚酰胺复合材料，其特征在于：
所述结晶促进剂为一种有机成分和无机成分的细致粉末混合物。
5.根据权利要求1所述的聚苯硫醚/聚酰胺复合材料，其特征在于：
所述的热稳定剂为三甘醇双-3-(3-叔丁基-4-羟基-5-甲基苯基)丙烯腈、三(2，4-二叔丁基酚)亚磷酸酯的一种。
6.根据权利要求1所述的聚苯硫醚/聚酰胺复合材料，其特征在于：所述的玻璃纤维的直径为6-17微米。
7.根据权利要求1所述的聚苯硫醚/聚酰胺复合材料，其特征在于：所述的硅烷偶联剂为γ-氨丙基三乙氧基硅烷。
8.根据权利要求1至7中任一权利要求所述的聚苯硫醚/聚酰胺复合材料，其特征在于，它由以下配比的原料按重量百分比配制而成：
聚苯硫醚(PPS) 44-55％
聚酰胺(PA) 15-25％
玻璃纤维(GF) 25-35％
热稳定剂 0.2-0.4％
硅烷偶联剂 0.1-0.4％
加工润滑剂 0.2-0.4％
结晶促进剂 0.2-0.4％。
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