CN111499938B - 一种炭黑配方橡胶连续混炼方法和装置 - Google Patents

一种炭黑配方橡胶连续混炼方法和装置 Download PDF

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CN111499938B
CN111499938B CN202010293048.1A CN202010293048A CN111499938B CN 111499938 B CN111499938 B CN 111499938B CN 202010293048 A CN202010293048 A CN 202010293048A CN 111499938 B CN111499938 B CN 111499938B
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汪传生
朱东林
边慧光
肖鑫鑫
宋凤鹏
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Qingdao University of Science and Technology
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Abstract

本发明属于橡胶连续混炼技术领域，具体涉及一种炭黑配方橡胶连续混炼方法和装置，将湿法混炼工艺与连续混炼进行结合，基于炭黑配方橡胶连续混炼装置实现，具体工艺过程包括制备炭黑浆料、制备助剂水溶液、制备助剂/炭黑母炼胶和连续混炼共四个步骤，通过机械研磨将填料和小料制备成均匀的分散溶液，与胶乳混合后，慢速搅拌使胶乳和炭黑或其他填料充分接触，利用高温雾化法将天然胶乳絮凝干燥，并使填料和小料均匀的被包裹在橡胶中，最后通过一段式低温连续混炼机进行补充混炼，制备的炭黑橡胶不仅物理性能和动态力学性能较常规干法混炼的炭黑橡胶有显著提高，而且生产周期也得到了缩短，并使填料在天然橡胶中达到了微观分散的效果。

Description

一种炭黑配方橡胶连续混炼方法和装置
技术领域：
本发明属于橡胶连续混炼技术领域，具体涉及一种炭黑配方橡胶连续混炼方法和装置，能够缩短生产周期，并使填料在天然橡胶中达到均匀分布和分散，具有连续性强、生产效率高、绿色环保和耗能低等优势。
背景技术：
混炼是橡胶产品加工过程中最为关键的工序，目的是将配方内的橡胶助剂与橡胶充分混合，并使橡胶助剂尽可能的分散均匀，与其说混炼结果的好坏直接决定着橡胶制品的性能和使用寿命，不如说橡胶助剂在橡胶中的分散和分布情况决定橡胶制品的性能和使用寿命，所以如何提高填料及助剂在橡胶基体中分散和分布以及能够实现连续混炼一直备受行业广泛关注。
目前，橡胶工业中的传统混炼方式是沿用密炼机多段式混炼方法，但是由于橡胶具有粘弹性与其他高聚物不同，导致橡胶在混炼过程中因被不断地剪切而温升较快，为防止胶料焦烧影响橡胶加工安全，混炼过程非常短暂，导致橡胶助剂在橡胶中的分散很难达到理想状态；为了提高混炼效率，橡胶行业开发出新的混炼方法和工艺，包括低温一次法、串联式混炼和连续混炼等。例如：中国专利201710312879.7公开的提高炭黑在母炼胶中分散均匀度的混炼方法按重量份计步骤如下：(1)参数设置：启动密炼机，设置密炼机的转子转速为54～56rpm，上顶栓压力为0.4～0.6MPa，混炼室温度为50～55℃，转子温度为50～55℃，排胶温度为155～165℃；(2)炭黑和生胶投料：取60～90份炭黑投入步骤(1)所述密炼机中，然后继续加入100份生胶，压下上顶栓，在混炼室利用转子旋转进行混炼40～50s，上顶栓浮使胶料翻转；(3)配料投放：在步骤(2)所述混炼室中继续投入母胶药品，具体为氧化锌1～5份、硬脂酸0.5～4份和防老剂1～6份，压下上顶栓进行混炼20～30s，提起上顶栓，使混炼室内的胶料充分翻转，即完成整个混炼过程，得到母炼胶。
虽然新的混炼技术能提高混炼效率和质量，但由于橡胶的本质特性仍然使得填料在混炼胶的分散等级达不到人们的期望，尤其是传统混炼工艺制备的炭黑/天然橡胶复合材料，其主要由于炭黑表面基团和结构特性，导致传统混炼时无法填充高份数炭黑和在混炼时容易填料发生团聚；其次，目前的连续混炼技术对胶料有较多的要求，多适用于粒(粉)状预制母胶的混炼，还存在胶料与配合剂配比难以保证等现象；最后，现有连续混炼技术和设备生产过程仍存在间歇性，将会对连续混炼效率打折扣。
为了突破混炼工艺的桎梏，湿法混炼工艺应运而生，将制备成浆料的橡胶助剂与天然胶乳混合搅拌、絮凝干燥，制备成母胶进行混炼，其液态混合的优势能大大提高橡胶混炼质量。例如：中国专利201710839208.6公开的一种湿法混炼制备炭黑母胶的方法包括以下步骤：选用表面活性剂处理炭黑制备分散均匀的炭黑浆液，在转速300～600m/min下搅拌20～60min制备得到炭黑浆液；将橡胶胶乳加入炭黑浆液在转速100～300m/min搅拌20～50min，将胶乳和炭黑絮出，过滤，干燥；其中，所述炭黑浆液的质量百分数为2～8％；所述表面活性剂为正丁醇、葡萄糖、聚乙二醇、脂肪醇聚氧乙烯醚-9、十二烷基硫酸钠、十二烷基苯磺酸钠中的至少一种；以橡胶胶乳中干胶质量为100份计，炭黑的加入量为30～80份，表面活性剂加入量为1～5份；中国专利201210266788.1公开的一种制备天然橡胶/炭黑–纳米二氧化硅混炼胶的湿炼法是在净水中加入炭黑，通过搅拌将炭黑分散于水中，形成炭黑在水中的质量百分比浓度为4％～10％的分散体；在净水中加入硅溶胶，通过搅拌将硅溶胶溶于水中，制成SiO2质量百分比浓度为10％～30％的硅溶胶水溶液；将炭黑分散体与硅溶胶水溶液共混，搅拌均匀，制成不含分散剂的炭黑–硅溶胶分散体C。
研究发现湿法混炼工艺虽然能够改善填料的微观分散程度，但是目前湿法工艺仍然采用成熟的强酸絮凝方式，酸性残留不仅对胶料制品产生影响，而且对设备以及操作人员身体健康都有危害，绿色环保性不强；后续混炼工艺还仍然使用传统的混炼工艺，即沿用密炼机多段式混炼方，生产连续性不强、自动化程度不高以及存在高能耗等。因此，研发一种针对高填充炭黑配方、以湿法工艺为基础和高效环保的连续混炼方法和装置，有良好的社会和应用前景。
发明内容：
本发明的目的在于克服现有技术存在的缺点，研发设计一种炭黑配方橡胶连续混炼方法和装置，无需进行硅烷反应，具有连续化生产程度高、节能环保以及填料高填充和高分散的优势。
为了实现上述目的，本发明涉及的一种炭黑配方橡胶连续混炼方法是基于炭黑配方橡胶连续混炼装置实现的，其工艺过程包括制备炭黑浆料、制备助剂水溶液、制备助剂/炭黑母炼胶和连续混炼共四个步骤：
(1)制备炭黑浆料：在1号烧杯中加入45质量份牌号为N110的炭黑和135g去离子水配制成质量百分比浓度为25wt％的炭黑水溶液，然后加入1g十二烷基苯磺酸钠作为活性剂，混合形成浆料，以750w的频率超声5min，研磨0-6h，得到炭黑浆料，备用；
(2)制备助剂水溶液：在2号烧杯中加入8质量份SiO2(二氧化硅)、1.5质量份4020(防老剂)、2质量份SAD(硬脂酸)、3.5质量份ZnO(氧化锌)、1质量份RD(防老剂)和去离子水配成质量百分比浓度为25wt％的助剂水溶液，研磨0-6h，备用；
(3)制备助剂/炭黑母炼胶：将133.2g步骤(1)制备的炭黑水浆料、116g步骤(2)制备的助剂水溶液与166.67质量份质量百分比浓度为60wt％的NRL(天然胶乳)混合，装入储存罐后泵送至搅拌罐进行搅拌形成混合溶液，搅拌频率为10Hz，通过喷射雾化形式将混合溶液絮凝干燥，喷射压力为1.2MPa，干燥温度为110-160℃，得到助剂/炭黑母炼胶；
(4)连续混炼：将步骤(3)制备的助剂/炭黑母炼胶、1质量份微晶蜡(Ceresinewax)和1质量份HTK(组氨酸-色氨酸-酮戊二酸盐液)投入第一阶段混炼机中进行混炼，混炼温度为130℃，转速为35r/min，混炼5-8分钟后，加入1.6质量份促进剂(NS)和1.9质量份硫磺(S)投入第二阶段混炼机中混炼，混炼温度为115℃，转速为35r/min，混炼5-8分钟后，得到炭黑配方橡胶。
本发明与现有技术相比，将湿法混炼工艺与连续混炼进行结合，基于炭黑配方橡胶连续混炼装置实现，具体工艺过程包括制备炭黑浆料、制备助剂水溶液、制备助剂/炭黑母炼胶和连续混炼共四个步骤，通过机械研磨将填料和小料制备成均匀的分散溶液，与胶乳混合后，慢速搅拌使胶乳和炭黑或其他填料充分接触，利用高温雾化法将天然胶乳絮凝干燥，并使填料和小料均匀的被包裹在橡胶中，最后通过一段式低温连续混炼机进行补充混炼，制备的炭黑橡胶不仅物理性能和动态力学性能较常规干法混炼的炭黑橡胶有显著提高，而且生产周期也得到了缩短，并使填料在天然橡胶中达到了微观分散的效果；其没有使用酸，减少了污染，避免了酸性残留对橡胶性能的影响，能够缩短生产周期，并使填料在天然橡胶中达到均匀分布和分散，提升橡胶性能。
附图说明：
图1为本发明涉及的炭黑配方橡胶连续混炼装置的主体结构原理示意图。
图2为本发明涉及的机筒的剖面结构原理示意图。
图3为本发明涉及的机头的主体结构原理示意图。
图4为本发明涉及的混炼转子的主体结构原理示意图。
图5为本发明涉及的混炼转子的剖面结构原理示意图。
图6为本发明涉及的机筒流道的排布示意图。
具体实施方式：
下面通过实施例并结合附图做进一步说明。
实施例1：
本实施例涉及的一种炭黑配方橡胶连续混炼方法是基于炭黑配方橡胶连续混炼装置实现的，其工艺过程包括制备制备炭黑浆料、制备助剂水溶液、制备助剂/炭黑母炼胶和连续混炼共四个步骤：
(1)制备炭黑浆料：在1号烧杯中加入45质量份牌号为N110的炭黑和135g去离子水配制成质量百分比浓度为25wt％的炭黑水溶液，然后加入1g十二烷基苯磺酸钠作为活性剂，混合形成浆料，以750w的频率超声5min，研磨4h，得到炭黑浆料，备用；
(2)制备助剂水溶液：在2号烧杯中加入8质量份SiO2(二氧化硅)、1.5质量份4020(防老剂)、2质量份SAD(硬脂酸)、3.5质量份ZnO(氧化锌)、1质量份RD(防老剂)和去离子水配成质量百分比浓度为25wt％的助剂水溶液，研磨4h，备用；
(3)制备助剂/炭黑母炼胶：将133.2g步骤(1)制备的炭黑水浆料、116g步骤(2)制备的助剂水溶液与166.67质量份质量百分比浓度为60wt％的NRL(天然胶乳)混合，装入储存罐1后泵送至搅拌罐3进行搅拌形成混合溶液，搅拌频率为10Hz，通过喷射雾化形式将混合溶液絮凝干燥，喷射压力为1.2MPa，干燥温度为135℃，得到助剂/炭黑母炼胶；
(4)连续混炼：将步骤(3)制备的助剂/炭黑母炼胶、1质量份微晶蜡(Ceresinewax)和1质量份HTK(组氨酸-色氨酸-酮戊二酸盐液)投入第一阶段混炼机10中高温/高剪切混炼，混炼温度为130℃，转速为35r/min，混炼5-8分钟后，加入1.6质量份促进剂(NS)和1.9质量份硫磺(S)投入第二阶段混炼机12中进行低温混炼，混炼温度为115℃，转速为35r/min，混炼5-8分钟后，得到炭黑配方橡胶。
本实施例涉及的炭黑配方橡胶连续混炼装置的主体结构包括储存罐1、研磨机2、搅拌罐3、泵4、搅拌器5、喷枪6、高温雾化罐7、一号失重称8、二号失重称9、第一阶段混炼机10、三号失重称11和第二阶段混炼机12；两台独立设置的储存罐1分别与研磨机2连接，研磨机2与搅拌罐3管道式连接，研磨机2与搅拌罐3之间设置有泵4，搅拌罐3内设置有搅拌器5，搅拌罐3的出口端与喷枪6连接，喷枪6伸入高温雾化罐7内，高温雾化罐7的下方设置有一号失重称8和二号失重称9，一号失重称8和二号失重称9的下方设置有第一阶段混炼机10，第一阶段混炼机10一侧设置有三号失重称11，第一阶段混炼机10和三号失重称11的下方设置有第二阶段混炼机12。
本实施例涉及的第一阶段混炼机10和第二阶段混炼机12的主体结构相同，均包括电机100、机筒101、机头102和混炼转子103；电机100与机筒101连接，机筒101与机头102螺栓式连接，机筒101内设置有双螺杆结构的混炼转子103。
本实施例涉及的研磨机2为球磨机或砂磨机，对物料进行研磨和混合；喷枪6为口径直径为0.5-5mm的气动喷枪；电机100为单入双输出结构的减速电机；机筒101采用两段或三段式结构，机筒101之间螺栓式连接，每段机筒101的内壁均开设有供温控介质循环的机筒流道104，每段机筒101的温度根据工艺要求设定；机头102的内壁开设有供温控介质循环的机头流道105，机头102的胶料挤出口呈倒锥形；温控介质为导热油，温控范围0-200℃，精确度为±0.5℃；混炼转子103为双螺杆混炼转子，具有啮合、剪切和输送胶料作用。
本实施例制备的炭黑配方橡胶的机械性能与常规干法制备的炭黑配方橡胶的机械性能的对比结果如下表：
序号 测试项目 常规干法 本实施例
1 硬度(邵氏A) 63 61
2 10％定伸(Mpa) 0.55 0.55
3 50％定伸(Mpa) 1.2 1.23
5 100％定伸(Mpa) 1.74 1.89
5 200％定伸(Mpa) 3.64 4.8
6 300％定伸(Mpa) 7.09 9.97
7 M300％/M100％ 3.16 3.44
8 M300％/M50％ 4.07 5.23
9 拉伸强度(Mpa) 24.34 29.73
10 扯断伸长率(％) 696.68 607.1
，可知：二者的硬度、10％定伸和50％定伸相差不大，本实施例制备的炭黑配方橡胶的100％定伸、300％定伸和M300％/M100％均高于常规干法制备的炭黑配方橡胶的100％定伸、300％定伸和M300％/M100％，本实施例制备的炭黑配方橡胶的拉伸强度相较于常规干法制备的炭黑配方橡胶的拉伸强度提高了22％，综合来看，本实施例制备的炭黑配方橡胶的机械性能优于常规干法制备的炭黑配方橡胶的机械性能。

Claims (2)

1.一种炭黑/橡胶连续混炼方法，其特征在于基于炭黑配方橡胶连续混炼装置实现的，其工艺过程包括制备炭黑浆料、制备助剂水溶液、制备助剂/炭黑母炼胶和连续混炼共四个步骤：
（1）制备炭黑浆料：在1号烧杯中加入45质量份牌号为N110的炭黑和135g去离子水配制成质量百分比浓度为25wt%的炭黑水溶液，然后加入1g十二烷基苯磺酸钠作为活性剂，混合形成浆料，以750w的频率超声5min，研磨0-6h，得到炭黑浆料，备用；
（2）制备助剂水溶液：在2号烧杯中加入8质量份SiO2、1.5质量份4020、2质量份SAD、3.5质量份ZnO、1质量份RD和去离子水配成质量百分比浓度为25wt%的助剂水溶液，研磨0-6h，备用；
（3）制备助剂/炭黑母炼胶：将133.2g步骤（1）制备的炭黑水浆料、116g步骤（2）制备的助剂水溶液与166.67质量份质量百分比浓度为60wt%的NRL混合，装入储存罐后泵送至搅拌罐进行搅拌形成混合溶液，搅拌频率为10Hz，通过喷射雾化形式将混合溶液絮凝干燥，喷射压力为1.2MPa，干燥温度为110-160℃，得到助剂/炭黑母炼胶；
（4）连续混炼：将步骤（3）制备的助剂/炭黑母炼胶、1质量份微晶蜡和1质量份HTK投入第一阶段混炼机中进行混炼，混炼温度为130℃，转速为35r/min，混炼5-8分钟后，加入1.6质量份促进剂和1.9质量份硫磺投入第二阶段混炼机中混炼，混炼温度为115℃，转速为35r/min，混炼5-8分钟后，得到炭黑配方橡胶。
2.根据权利要求1所述的炭黑/橡胶连续混炼方法，其特征在于，炭黑/橡胶连续混炼装置的主体结构包括储存罐、研磨机、搅拌罐、泵、搅拌器、喷枪、高温雾化罐、一号失重称、二号失重称、第一阶段混炼机、三号失重称和第二阶段混炼机；两台独立设置的储存罐分别与研磨机连接，研磨机与搅拌罐管道式连接，研磨机与搅拌罐之间设置有泵，搅拌罐内设置有搅拌器，搅拌罐的出口端与喷枪连接，喷枪伸入高温雾化罐内，高温雾化罐的下方设置有一号失重称和二号失重称，一号失重称和二号失重称的下方设置有第一阶段混炼机，第一阶段混炼机一侧设置有三号失重称，第一阶段混炼机和三号失重称的下方设置有第二阶段混炼机；第一阶段混炼机和第二阶段混炼机的主体结构相同，均包括电机、机筒、机头和混炼转子；电机与机筒连接，机筒与机头螺栓式连接，机筒内设置有双螺杆结构的混炼转子；研磨机为球磨机或砂磨机，对物料进行研磨和混合；喷枪为口径直径为0.5-5mm的气动喷枪；电机为单入双输出结构的减速电机；机筒采用两段或三段式结构，机筒之间螺栓式连接，每段机筒的内壁均开设有供温控介质循环的机筒流道，每段机筒的温度根据工艺要求设定；机头的内壁开设有供温控介质循环的机头流道，机头的胶料挤出口呈倒锥形；温控介质为导热油，温控范围0-200℃，精确度为±0.5℃；混炼转子为双螺杆混炼转子，具有啮合、剪切和输送胶料作用。
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