CN101418121A - 一种低熔点尼龙6及其制备方法 - Google Patents
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Abstract
本发明公开了一种低熔点尼龙6及其制备方法，按照重量份计算，本发明低熔点尼龙6是由普通尼龙6 92～ 98份、氯化钙2～8份、催化剂0.01～0.03份和加工助剂0.1～0.2份制备而成。按比例将所述原料混合均匀，按照聚合物加工成形的方法在双螺杆挤出机中挤出成型并造粒即得低熔点尼龙6，其中双螺杆挤出机的螺杆温度为240～270℃，螺杆转速为160～180转/分钟。本发明采用氯化钙对普通尼龙6进行络合改性，降低了原料的成本，制备出的低熔点尼龙6在加工流动性、力学性能等方面与杜邦公司的同类产品接近，可以与PVC等加工温度较低的聚合物实现共混，且本发明方法简单，易操作，非常适合在产业上推广应用。
Description
技术领域
本发明涉及一种低熔点尼龙6及其制备方法，特别是涉及通过金属氯化物熔融挤出对普通尼龙6进行络合改性而制备的低熔点尼龙6及其熔融挤出改性方法。
背景技术
尼龙6(PA6)具有机械强度高、韧性好、电气性能佳、耐磨、耐油、耐弱酸碱等一系列优异性能，是一种应用广泛的工程塑料。PA6不仅能作为基体树脂，用聚烯烃、橡胶弹性体、无机刚性粒子及聚醚、聚酯、聚酰亚胺等其他工程塑料对其改性，使其具有高抗冲击性、低吸水性和良好的加工性能，也能作为聚合物合金的第二组份，增韧增强聚丙烯、聚碳酸酯等其它聚合物或者制备阻隔材料。
普通尼龙6的加工温度较高，由于加工温度之间的矛盾，很难实现普通尼龙6对PVC等加工温度较低的聚合物进行共混改性。通过溶液法采用锂、锌等金属离子和尼龙中的酰胺基团的相互作用，破坏高分子体系的氢键结构，使尼龙6的结晶度减小，结晶规整度降低，因而降低尼龙6的熔点。但溶液法虽然可以降低尼龙6的熔点，制备低熔点尼龙6，但由于生产成本高、工艺复杂等原因，只限于实验室制备，很难实现产业化。
发明内容
本发明所要解决的技术问题是提供一种利用金属氯化物对普通尼龙6进行络合改性制备的低熔点尼龙6及其熔融挤出制备方法，应用金属氯化物来制备低熔点尼龙6的生产成本低，生产工艺简单，制备的低熔点尼龙6的熔程在145℃～215℃之间，可以与PVC等加工温度较低的聚合物实现共混。
本发明机理：金属氯化物能和尼龙6分子链上的羰基发生络合配位作用而插入尼龙6分子链，破坏尼龙6的氢键，降低尼龙6分子链的规整排列，使尼龙6的结晶规整度降低和结晶度减小，从而降低尼龙6的熔点。经金属氯化物熔融挤出络合改性制备的低熔点尼龙6可以实现与PVC等加工温度较低的聚合物共混加工。
为了解决上述技术问题，依据上述机理，本发明采用如下的技术方案：
按照重量份计算，低熔点尼龙6是由普通尼龙692～98份、金属氯化物2～8份、催化剂0.01～0.03份和加工助剂0.1～0.2份制备而成。
其中，金属氯化物选用氯化钙，催化剂为过渡金属卤化物，加工助剂为丙三醇或硼酸。加入催化剂的作用是加速钙离子与羰基的配位，加工助剂的作用为进一步促进尼龙6和氯化钙的络合反应。
前述低熔点尼龙6的制备方法：按比例取普通尼龙6、金属氯化物、催化剂和加工助剂混合均匀，按照聚合物加工成形的方法在双螺杆挤出机中挤出成型并造粒即得低熔点尼龙6。
其中双螺杆挤出机的螺杆温度为200～270℃，螺杆转速为160～240转/分钟。在将原料混合均匀制备低熔点尼龙6前，先将氯化钙在100～130℃干燥10～15小时后粉碎细化。聚合物在双螺杆挤出机中挤出成型的时间是有限的，粉碎后可以使氯化钙均匀分散，加快反应速度，缩短反应时间，达到反应挤出的目的。
按照前述配方和方法制备出的低熔点尼龙6的熔程在145℃～215℃之间，缺口冲击强度为5～10KJ/m2，拉伸强度为60～85MPa，硬度为普通尼龙6硬度的1～1.5倍。从普通尼龙6和低熔点尼龙6的差示扫描热分析(DSC)曲线可以看出低熔点尼龙6的熔点小于普通尼龙6的熔点(228℃)，其加工温度大大降低。起始熔融温度由普通尼龙6的211℃下降到145℃～170℃左右。
与现有制备低熔点尼龙6的方法相比，本发明是采用金属氯化物对普通尼龙6进行络合改性，制备出的低熔点尼龙6的熔程为150～210℃之间，缺口冲击强度为5～10KJ/m2，拉伸强度为60～80MPa，硬度为普通尼龙6硬度的1～1.5倍，其在加工流动性、力学性能等方面与杜邦公司的同类产品接近，可以与PVC等加工温度较低的聚合物实现共混，但其生产成本却很低，有重要的应用前景。且本发明方法简单，易操作，非常适合在产业上推广应用。
具体实施方式
本发明的优选实施方式：氯化钙在120℃下真空干燥机中干燥10小时，然后用高速搅拌机粉碎细化，按照重量配比称取普通尼龙695Kg、氯化钙5Kg、催化剂三氯化铁0.03Kg和加工助剂丙三醇0.15Kg，将普通尼龙6颗粒、氯化钙、三氯化铁和丙三醇混合均匀，按照聚合物加工成形的方法在双螺杆挤出机中挤出成型并造粒即得低熔点尼龙6，其中双螺杆挤出机的螺杆温度为200～270℃，螺杆转速为160～240转/分钟。在上述配方和工艺的范围内，不同配比体系的优化工艺不同，表1给出了优化工艺实验制得的典型低熔点尼龙6的性能指标。
表1典型低熔点尼龙6的性能指标
表注：熔程和熔点采用GB/T19466方法绘制DSC曲线得到；缺口冲击强度采用ASTM D-256方法在23℃测得；拉伸强度采用ASTM D-638方法在23℃测得；弯曲强度采用ASTM D-790方法在23℃测得；硬度采用GB934288方法在23℃测得。
Claims (7)
- 【权利要求1】一种低熔点尼龙6，其特征在于：按照重量份计算，它是由普通尼龙692～98份、金属氯化物2～8份、催化剂0.01～0.03份和加工助剂0.1～0.2份制备而成。
- 【权利要求2】按照权利要求1所述的低熔点尼龙6，其特征在于：所述金属氯化物为氯化钙。
- 【权利要求3】按照权利要求1所述的低熔点尼龙6，其特征在于：所述催化剂为过渡金属卤化物。
- 【权利要求4】按照权利要求1所述的低熔点尼龙6，其特征在于：所述加工助剂为丙三醇或硼酸。
- 【权利要求5】一种如权利要求1—4任一所述的低熔点尼龙6的制备方法，其特征在于：取普通尼龙6、金属氯化物、催化剂和加工助剂混合均匀，按照聚合物加工成形的方法在双螺杆挤出机中挤出成型并造粒即得低熔点尼龙6。
- 【权利要求6】按照权利要求5所述低熔点尼龙6的制备方法，其特征在于：所述双螺杆挤出机的螺杆温度为200～270℃，螺杆转速为160～240转/分钟。
- 【权利要求7】按照权利要求5所述低熔点尼龙5的制备方法，其特征在于：混合前将金属氯化物在100～130℃干燥10～15小时后粉碎细化。
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102766943A (zh) * | 2012-06-27 | 2012-11-07 | 吴江亚太化纺有限公司 | 一种远红外尼龙纤维纺丝工艺 |
| CN103910998A (zh) * | 2014-04-02 | 2014-07-09 | 合肥杰事杰新材料股份有限公司 | 一种低硬度尼龙6组合物及其制备方法 |
| CN104194327A (zh) * | 2014-08-19 | 2014-12-10 | 贵州省材料产业技术研究院 | 增强型微透明尼龙材料及其制备方法 |
| CN105822008A (zh) * | 2016-05-18 | 2016-08-03 | 南京旭华圣洛迪新型建材有限公司 | 一种高强度建筑墙板 |
| CN105820631A (zh) * | 2016-05-18 | 2016-08-03 | 南京旭华圣洛迪新型建材有限公司 | 一种耐腐蚀装饰面板 |
| CN106700522A (zh) * | 2016-12-15 | 2017-05-24 | 苏州博云塑业有限公司 | 一种具有低熔点易于成型的尼龙6复合材料及制备方法 |
| CN113214470A (zh) * | 2021-04-01 | 2021-08-06 | 华东理工大学 | 一种低熔点的聚丁内酰胺的制备方法 |
| CN114933701A (zh) * | 2022-06-06 | 2022-08-23 | 镇江市营房塑电有限公司 | 一种低温增韧mc尼龙6复合材料的制备方法 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS5894863A (ja) | 1981-11-30 | 1983-06-06 | 旭メデイカル株式会社 | 合成高分子重合体よりなる多孔膜 |
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| CN102766943A (zh) * | 2012-06-27 | 2012-11-07 | 吴江亚太化纺有限公司 | 一种远红外尼龙纤维纺丝工艺 |
| CN103910998A (zh) * | 2014-04-02 | 2014-07-09 | 合肥杰事杰新材料股份有限公司 | 一种低硬度尼龙6组合物及其制备方法 |
| CN104194327A (zh) * | 2014-08-19 | 2014-12-10 | 贵州省材料产业技术研究院 | 增强型微透明尼龙材料及其制备方法 |
| CN105822008A (zh) * | 2016-05-18 | 2016-08-03 | 南京旭华圣洛迪新型建材有限公司 | 一种高强度建筑墙板 |
| CN105820631A (zh) * | 2016-05-18 | 2016-08-03 | 南京旭华圣洛迪新型建材有限公司 | 一种耐腐蚀装饰面板 |
| CN106700522A (zh) * | 2016-12-15 | 2017-05-24 | 苏州博云塑业有限公司 | 一种具有低熔点易于成型的尼龙6复合材料及制备方法 |
| CN106700522B (zh) * | 2016-12-15 | 2019-04-09 | 江苏博云塑业股份有限公司 | 一种具有低熔点易于成型的尼龙6复合材料及制备方法 |
| CN113214470A (zh) * | 2021-04-01 | 2021-08-06 | 华东理工大学 | 一种低熔点的聚丁内酰胺的制备方法 |
| CN114933701A (zh) * | 2022-06-06 | 2022-08-23 | 镇江市营房塑电有限公司 | 一种低温增韧mc尼龙6复合材料的制备方法 |
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