CN105330985B - 一种三元乙丙橡胶发泡型材的盐浴硫化工艺 - Google Patents
一种三元乙丙橡胶发泡型材的盐浴硫化工艺 Download PDFInfo
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Abstract
本发明涉及一种橡胶材料生产工艺，特别涉及一种三元乙丙橡胶发泡型材的盐浴硫化工艺。一种三元乙丙橡胶发泡型材的盐浴硫化工艺，该工艺包括如下步骤：取发泡原料机械混合后，经挤出机挤出成型，盐浴槽硫化发泡后，制得三元乙丙橡胶发泡型材；所述的发泡原料包括三元乙丙橡胶、环烷油、炭黑、碳酸钙、硬酯酸、氧化锌、硫磺、促进剂二烷基二硫代氨基甲酸盐、偶氮二甲酰胺。本发明采用了挤出成型‑盐浴硫化连续生产工艺，降低了生产成本，提高了生产效率。
Description
技术领域
本发明涉及一种橡胶材料生产工艺，特别涉及一种三元乙丙橡胶发泡型材的盐浴硫化工艺。
背景技术
橡胶发泡材料相对普通密实橡胶材料而言，最一般的共同特点是密度小，质量轻，比面积大，能量吸收能力强，阻尼、隔音以及隔热性能好，美观实用等一系列优点，已在工业、农业、建筑、交通运输、军工、航空航天、日用品等领域获得了广泛的应用。如用于密封，保温隔热，防振防撞，隔音等诸多场合。在科学技术研究与国民经济建设中发挥着巨大的作用，已成为人们生产和生活中不可缺少的材料。
三元乙丙橡胶（EPDM）是由乙烯、丙烯以及少量的第三单体共聚而成的橡胶，它的主链上由化学稳定的饱和烃组成，只在侧链中含有不饱和双键，分子内无极性取代基，分子内聚能低，分子链段在较宽的温度范围内保持柔性。因而具有优异的化学稳定性，耐老化性、耐化学药品性、电绝缘性，冲击弹性和低温性能，以及耐热水性能等。为此，EPDM在橡胶制品工业中获得越来越广泛的应用，主要用于汽车零件、电器制品、工业制品、建筑材料和家庭用品及塑料改性剂等许多方面，其发泡材料则广泛用于制造汽车的挡风条，缓冲胶垫，建筑工程用密封垫片，弱电部件的绝热材料、减振材料、简易的潜水服及鞋等制品。
目前国内EPDM发泡型材都是采用预硫化加-次硫化的工艺(两步模压法)生产，但产品的篇幅较小且不能连续化生产，在生产过程为满足预硫化和硫化发泡的温度、体积要求，需多次更换模具，生产周期需要半个小时，生产效率很低，而且中间更换模具会造成制品温度的变化，影响最终橡胶发泡板材的品质。国际上只有意大利、日本等国家推出了橡胶发泡板材发泡硫化连续生产线，但价格非常昂贵，维护成本非常高。EPDM发泡型材虽然性能优异，但由于生产成本和生产效率的等原因，限制了其工业化生产。采用盐浴硫化-发泡工艺，制备的EPDM发泡型材发泡均匀，形成闭孔结构，隔热性和隔音性好，篇幅较大，生产速度很高，有利于其在建筑保温、汽车配件、防水材料、电线电缆、空调制冷、军工器械等行业的应用推广。
发明内容
本发明针对现有技术的缺陷，提供一种三元乙丙橡胶发泡型材的盐浴硫化工艺，该工艺实现了三元乙丙橡胶发泡型材的连续生产，缩短了生产时间。
本发明解决其技术问题所采用的技术方案是：
一种三元乙丙橡胶发泡型材的盐浴硫化工艺，该工艺包括如下步骤：取发泡原料机械混合后，经挤出机挤出成型，盐浴槽硫化发泡后，制得三元乙丙橡胶发泡型材；所述的发泡原料包括三元乙丙橡胶、环烷油、炭黑、碳酸钙、硬酯酸、氧化锌、硫磺、促进剂二烷基二硫代氨基甲酸盐、偶氮二甲酰胺。
作为优选，将三元乙丙橡胶放入双辊混炼机上塑炼3分钟，分别加入环烷油、炭黑、碳酸钙、硬酯酸、氧化锌混炼10分钟，再加入硫磺、促进剂二烷基二硫代氨基甲酸盐、AC混合均匀，薄通10次后下料得到三元乙丙橡胶预混物；然后三元乙丙橡胶预混物再经单螺杆挤出机挤出成型，在牵引机的作用下经盐浴槽硫化发泡后，制得三元乙丙橡胶发泡型材。
作为优选，所述的发泡原料由以下重量份的组分组成：100份三元乙丙橡胶、10~50份环烷油、5~40份炭黑、5~30份碳酸钙、0.5~3.0份硬酯酸、1.0~5.0份氧化锌、2.0~8.0份硫磺、1.0~5.0份促进剂二烷基二硫代氨基甲酸盐、1.0~5.0份偶氮二甲酰胺（AC）。
作为优选，所述的促进剂二烷基二硫代氨基甲酸盐选自二甲基二硫代氨基甲酸锌（PZ）、二乙基二硫代氨基甲酸锌（ZDEC）、二丁基二硫代氨基甲酸锌（BZ）、乙基苯基二硫代氨基甲酸锌（PX）。
作为优选，所述的单螺杆挤出机各段温度控制在50～110℃，其中加料段温度为50～60℃，口模温度为90～110℃。
作为优选，所述的盐浴槽中熔盐的温度控制在180～220℃，物料在盐浴槽的停留时间为3~8分钟。
与现有技术相比，本发明的有益效果体现在如下几方面：
1、本发明制得的三元乙丙橡胶发泡型材，所用的硫化-发泡体系为硫磺/二烷基二硫代氨基甲酸盐/偶氮二甲酰胺，其中硫化剂为硫磺，促进剂为二烷基二硫代氨基甲酸盐，发泡剂为偶氮二甲酰胺，促进剂二烷基二硫代氨基甲酸盐不仅加速三元乙丙橡胶的硫化，而且导致偶氮二甲酰胺活化降低其分解温度，提高偶氮二甲酰胺的分解速率，使三元乙丙橡胶硫化和发泡过程形成很好的匹配；
2、本发明采用了盐浴硫化发泡工艺，制备的型材发泡均匀，形成闭孔结构，尺寸稳定性好；
3、本发明采用了挤出成型-盐浴硫化连续生产工艺，降低了生产成本，提高了生产效率。
具体实施方式
下面通过具体实施例，对本发明的技术方案作进一步的具体说明。应当理解，本发明的实施并不局限于下面的实施例，对本发明所做的任何形式上的变通和/或改变都将落入本发明保护范围。
在本发明中，若非特指，所有的份、百分比均为重量单位，所采用的设备和原料等均可从市场购得或是本领域常用的。下述实施例中的方法，如无特别说明，均为本领域的常规方法。
实施例1
将100份三元乙丙橡胶放入双辊混炼机上塑炼3分钟，50份环烷油、40份炭黑、5份碳酸钙、0.5份硬酯酸、1.0份氧化锌混炼10分钟，再加入8.0份硫磺、5.0份促进剂PZ、5.0份AC混合均匀，薄通10次后下片，制得三元乙丙橡胶预混物，然后三元乙丙橡胶预混物再经单螺杆挤出机挤出成型，其中单螺杆挤出机各段温度控制在50～110℃，其中加料段温度为50～60℃，口模温度为90～110℃，在牵引机的作用下经180℃盐浴槽硫化发泡8分钟，制得三元乙丙橡胶发泡型材。
实施例2
三元乙丙橡胶发泡型材的制备操作同实施例1。三元乙丙橡胶发泡型材的配方为100份三元乙丙橡胶、10份环烷油、5份炭黑、30份碳酸钙、3.0份硬酯酸、5.0份氧化锌、2.0份硫磺、1.0份ZDEC、1.0份AC，盐浴槽中熔盐的温度为220℃，盐浴硫化时间为3分钟。
实施例3
三元乙丙橡胶发泡型材的制备操作同实施例1。三元乙丙橡胶发泡型材的配方为100份三元乙丙橡胶、20份环烷油、15份炭黑、20份碳酸钙、2.0份硬酯酸、2.0份氧化锌、6.0份硫磺、3.0份BZ、2.0份AC，盐浴槽中熔盐的温度为200℃，盐浴硫化时间为5分钟。
实施例4
三元乙丙橡胶发泡型材的制备操作同实施例1。三元乙丙橡胶发泡型材的配方为100份三元乙丙橡胶、30份环烷油、30份炭黑、10份碳酸钙、3.0份硬酯酸、3.0份氧化锌、6.0份硫磺、4.0份PX、4.0份AC，盐浴槽中熔盐的温度为190℃，盐浴硫化时间为6分钟。
作为比较，实施例1的三元乙丙橡胶发泡型材配方中促进剂PZ被相同份数的二硫化四甲基秋兰姆（TMTD）代替，硫化发泡在硫化床进行，硫化温度和时间与盐浴硫化工艺相同，所得三元乙丙橡胶发泡型材的性能测试和生产效率结果比较见表1。
表1
| 三元乙丙橡胶发泡型材I | 三元乙丙橡胶发泡型材II | |
| 密度（g/cm3） | 0.581 | 0.466 |
| 断裂强度 （MPa） | 7.62 | 7.70 |
| 断裂延伸率 （%） | 544 | 609 |
| 生产时间（分钟/100米） | 115 | 52 |
三元乙丙橡胶发泡型材I：配方为100份三元乙丙橡胶、50份环烷油、40份炭黑、5份碳酸钙、0.5份硬酯酸、1.0份氧化锌、8.0份硫磺、5.0份促进剂TMTD、5.0份AC；三元乙丙橡胶发泡型材II：配方和制备工艺同由实施例6。
从产品密度可以看出，相比硫磺/TMTD/AC，发明所用的硫磺/二烷基二硫代氨基甲酸盐/AC有效提高三元乙丙橡胶型材的发泡倍率，降低了橡胶型材比重，这主要是因为二烷基二硫代氨基甲酸盐中的锌离子外围电子排布为4S24P2具有空轨道，而发泡剂AC结构中N、O上皆有孤对电子，根据路易斯酸-碱配位原理，二者进行结合时，AC上的N、O原子上的孤对电子进入Zn2+的空轨道，同时-N-C-上的Л键上电子云流动，使-N-C-电子云浓度流向两边，中间重叠度减小，因而导致-N-C-键容易断裂，导致AC活化其分解温度降低。
从力学性能看，盐浴硫化制备的三元乙丙橡胶发泡型材的强度和延展性均优于传统硫化床制备的材料，这可归因于盐浴硫化制备的三元乙丙橡胶发泡型材的泡孔直径尺寸较小，分布比较均匀。从生产效率的角度看，采用盐浴硫化生产工艺制备三元乙丙橡胶发泡型材的生产速度要高于传统的硫化床生产工艺。
以上所述的实施例只是本发明的一种较佳的方案，并非对本发明作任何形式上的限制，在不超出权利要求所记载的技术方案的前提下还有其它的变体及改型。
Claims (4)
1.一种三元乙丙橡胶发泡型材的盐浴硫化工艺，其特征在于该工艺包括如下步骤：取发泡原料机械混合后，经挤出机挤出成型，盐浴槽硫化发泡后，制得三元乙丙橡胶发泡型材；所述的盐浴槽中熔盐的温度控制在180～220℃，物料在盐浴槽的停留时间为3~8分钟；所述的发泡原料由以下重量份的组分组成：100份三元乙丙橡胶、10~50份环烷油、5~40份炭黑、5~30份碳酸钙、0.5~3.0份硬酯酸、1.0~5.0份氧化锌、2.0~8.0份硫磺、1.0~5.0份促进剂二烷基二硫代氨基甲酸盐、1.0~5.0份偶氮二甲酰胺（AC）。
2.根据权利要求1所述的盐浴硫化工艺，其特征在于：将三元乙丙橡胶放入双辊混炼机上塑炼3分钟，分别加入环烷油、炭黑、碳酸钙、硬酯酸、氧化锌混炼10分钟，再加入硫磺、促进剂二烷基二硫代氨基甲酸盐、AC混合均匀，薄通10次后下料得到三元乙丙橡胶预混物；然后三元乙丙橡胶预混物再经单螺杆挤出机挤出成型，在牵引机的作用下经盐浴槽硫化发泡后，制得三元乙丙橡胶发泡型材。
3.根据权利要求1所述的盐浴硫化工艺，其特征在于：所述的促进剂二烷基二硫代氨基甲酸盐选自二甲基二硫代氨基甲酸锌（PZ）、二乙基二硫代氨基甲酸锌（ZDEC）、二丁基二硫代氨基甲酸锌（BZ）。
4.根据权利要求2所述的盐浴硫化工艺，其特征在于：所述的单螺杆挤出机各段温度控制在50～110℃，其中加料段温度为50～60℃，口模温度为90～110℃。
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