CN107936331B - 一种多阶螺杆连续脱硫制备再生橡胶的方法 - Google Patents

一种多阶螺杆连续脱硫制备再生橡胶的方法 Download PDF

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CN107936331B
CN107936331B CN201711102594.7A CN201711102594A CN107936331B CN 107936331 B CN107936331 B CN 107936331B CN 201711102594 A CN201711102594 A CN 201711102594A CN 107936331 B CN107936331 B CN 107936331B
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rubber powder
screw extruder
temperature
section
rubber
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CN107936331A (zh
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张立群
任冬云
史金炜
戈风行
陈成杰
汪冯新
王杰
张植俞
陆涛
刘晓博
杨晓彤
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Nanjing Lvjinren Rubber Hi Tech Co ltd
Beijing University of Chemical Technology
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Nanjing Lvjinren Rubber Hi Tech Co ltd
Beijing University of Chemical Technology
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Priority to US16/476,535 priority patent/US11453758B2/en
Priority to EP17931711.0A priority patent/EP3611221B8/en
Priority to PCT/CN2017/118796 priority patent/WO2019090938A1/zh
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Abstract

本发明涉及一种多阶螺杆连续脱硫制备再生橡胶的方法，属废旧橡胶循环再利用领域。初步混合的胶粉和软化剂经连续密闭保温输送计量装置，压实加入第一台异向双螺杆挤出机，在挤出机内温度的作用下软化剂均匀渗透废胶粉，废胶粉初步脱硫；经输送装置冷却后，对接进入第二台多螺杆挤出机内，通过活化剂和剪切作用实现快速脱硫再生；制备的脱硫胶粉经冷却输送装置，进入第三台串联的多螺杆挤出机内，在低温下通过剪切作用改善脱加工性能，挤出后通过成型装置和冷却装置，最终包装得到再生橡胶。整个流程在密闭隔氧条件下完成，实现了安全、简单、连续的脱硫再生，具有节能、环保的优点，所得再生胶性能优异。

Description

一种多阶螺杆连续脱硫制备再生橡胶的方法
技术领域
本发明涉及一种制备再生胶的新方法，尤其涉及多阶螺杆挤出机再生废橡胶的方法，属于废旧橡胶循环再利用领域。
背景技术
为了改善生胶的性能，需要对生胶进行硫化加工，生胶由线性高分子链交联形成三维网状结构，从而使胶料具备高强度、高弹性、高耐磨、抗腐蚀等特点，满足生产生活的需要。硫黄硫化体系是橡胶硫化最常用的方法之一，通过S-S键、C-S键连接高分子链形成交联网络。具有三维网状结构的热固性硫化橡胶制品达到使用寿命后，不溶不熔，难以进行处理，成为工业有害废弃物中危害最大的垃圾之一，2015年全球产生废轮胎高达4047万吨。制备再生胶可以达到循环利用橡胶的目的，受到广泛的重视，是中国废橡胶的最主要再利用方式，年产量超过450万吨，约占全球再生橡胶产量的80％。
目前，国际上关于废橡胶的断键再生机理主要有两种观点：1.化学键的键能差；2.化学键的弹性系数差。所谓化学键的键能差就是利用C-C键的键能大于C-S键和S-S键的键能，通过控制施加热的所用，使C-S键和S-S键断裂，而不使主链断裂。化学键的弹性系数差是指C-C键、C-S键、S-S键三者在剪切的作用下，利用弹性系数的不同，选择性断裂交联键。
通过化学键的键能差选择性的打断S-S键，在中国得到了广泛的应用，形成了以“高温高压动态脱硫”为主的脱硫再生工艺。将再生剂和水一起加入脱硫罐中，工作压力2.2MPa左右，工作温度约220℃，脱硫时间3小时左右，泄压得到脱硫胶粉。活化剂在软化剂的辅助下，渗透并进入废橡胶内部与之发生反应，破坏交联网络，使之准线性化、可再加工。但是高温条件下再生剂由外向内边渗透边反应的过程中，容易引起废胶粉内外脱硫程度不均匀，产生“核—壳”结构；同时搅拌转速慢，脱硫不均匀。为了避免胶粉表面过度脱硫引起力学性能的下降，脱硫胶粉的门尼粘度往往比较高，脱硫程度较低，需经3～4台高速精炼机多次过辊压炼，才能制备加工性能良好的再生胶。长时间的高温高压存在严重的安全隐患，间歇操作生产率低，罐壁结垢造成工艺不好控制；精炼机开放式的操作环境烟气大，环境污染严重，安全性差，脱硫程度低的脱硫胶粉导致能耗较高。
目前行业都积极改进传统的脱硫方式，高温高压动态脱硫罐逐渐被市场淘汰。王京东等(CN 103665428 B连续高温常压脱硫机)是将混有再生剂的废橡胶通过脱硫机内的螺旋输送装置，实现废橡胶的连续、密闭脱硫再生。通过提高脱硫温度达到300℃，将反应时间缩短至15～20min之间。但是由于螺旋结构无法压实物料，传热较差渗透慢，导致再生胶力学性能较差。吕柏源等(CN 103087349 A一种单螺杆热化学、强力剪切复合脱硫设备及其脱硫方法)通过在单螺杆机筒上添加销钉，调整螺纹元件，使得单螺杆出了保持热化学反应功能外，对脱硫的物料进行高剪切作用，强化热化学反应的脱硫效果。物料在单螺杆中并非一直处于压实状态，不可避免的混入氧气，高温条件下橡胶主链降解严重。张立群等(CN102977404B，一种双阶双螺杆挤出机连续制备再生胶的方法)等将废胶粉与再生剂于搅拌机内预处理后，在高温下静置使再生剂充分渗透溶胀胶粉，再加入异向双螺杆挤出机，取代传统的高温高压动态反应罐，脱硫胶粉进入同向双螺杆挤出机，在低温下施加高剪切的作用，取代精炼机。50℃～100℃条件下再生剂粘度仍很高，需要静置12h～36h才能完成渗透，间歇操作生产效率低，高温下保温时间长能耗大；在异向双螺杆内热量仍是由胶粉外部向内传递，不可避免的存在“核—壳”结构，导致力学性能不佳，同向双螺杆精炼过程中的能耗依然很大。
由于受到传热过程和渗透效果的影响，通过化学键的键能差很难实现均匀脱硫，容易产生“核壳”结构，国内外学者对利用化学键的弹性系数差选择性断裂交联键开展了大量工作，取得了很多成果。倪雪文等(CN102888030B废橡胶高温常压再生工艺)不添加任何软化剂和催化剂，直接将胶粉搅拌后通过强制喂料装置压入双螺杆挤出机中施加高温高剪切，实现快速脱硫反应，冷却后的物料加入到变频开放式炼胶机上进行快速剪切，随后在开放式炼胶机中精炼成型，最后经过滤胶后出片。不添加任何助剂的废胶粉粘度高，硬度大，双螺杆加热软化区的温度高达300～350℃才能使胶粉快速软化，不可避免的导致主链的降解，引起再生胶力学性能的下降。汪传生等(CN104004222B一种废橡胶低温连续再生装置及工艺方法)采用密炼机将废胶粉和再生剂进行初步混合解联后，加入双螺杆挤出机进行机械化学反应，通过输送带加入到开炼机上进行精炼，冷却后得到再生胶。开放式的输送装置和精炼设备，污染环境；密炼机间歇生产的物料从的出料口直接排到双螺杆挤出机的入口，导致会生产过程不稳定。利用化学键的弹性系数差控制合适的剪切可以选择性断裂脱硫，并不存在由于渗透不均匀导致“核壳”结构的问题。
发明内容：本发明的目的在于克服现有单独利用化学键的键能差或化学键的弹性系数差脱硫再生技术的不足，提出一种连续制备再生胶的方法，利用多阶螺杆连续脱硫制备再生橡胶。
本发明的是通过以下流程来实现的：一种多阶螺杆连续脱硫制备再生橡胶的方法，其特征在于该方法包括再生剂的渗透和废胶粉的初步脱硫、脱硫工序和精炼工序联动完成，将废胶粉与软化剂于搅拌机内60℃～120℃下处理5min～25min后，进入60℃～120℃的保温缓冲罐内，经连续密闭保温输送计量装置进入到一台异向双螺杆挤出机内，在100℃～340℃停留1min～6min完成软化剂向胶粉内部的均匀渗透和废胶粉的初步脱硫，再经连续冷却装置在密闭条件下冷却至40℃～80℃，得到门尼粘度为100～230的初步脱硫物料，然后经连续输送至计量加料装置，进入第二台多螺杆挤出机内，通过侧喂料装置加入活化剂，控制多螺杆挤出机的机筒和芯轴的温度在20℃～110℃，1min～6min完成脱硫反应由挤出机挤出门尼粘度为70～150脱硫胶粉，经连续冷却装置在密闭条件下冷却至25℃～60℃，进入第三台多螺杆挤出机内，控制多螺杆挤出机的机筒和芯轴的温度在-5℃～50℃，在剪切条件下精炼1～10min由挤出后，再经成型装置和冷却装置使物料冷却至50℃以下后完成精炼工序，最终包装即可得到所需再生橡胶产品。
废胶粉与软化剂、活化剂的质量比为100:(2～20)：(0.01～3)；
优选的软化剂是煤焦油、芳烃油、松焦油、妥尔油、环烷油、双戊烯、石蜡油、油酸、棉籽油、松香的一种或几者的混合物，活化剂是芳烃二硫化物、多烷基苯酚硫化物、苯基硫醇、胺基化合物的一种或几者的混合物。
所用的废胶粉是废载重子午线轮胎胶粉或废轿车胎胶粉的一种或二者的混合物。
所用的多螺杆挤出机是同向双螺杆挤出机或同向平行三螺杆挤出机中的一种。
优选的的异向双螺杆挤出机的加热排气段温度在120℃～200℃，保温段温度在200℃～340℃，冷却段温度在100℃～200℃。
优选的第二台多螺杆挤出机混合段的机筒温度在40℃～70℃，剪切段的机筒温度在70℃～90℃，冷却段机筒温度在30℃～60℃。
优选的第三台多螺杆挤出机第一物料输送段的机筒温度在0℃～25℃，预剪切段的机筒温度在5℃～40℃，第二物料输送段的机筒温度在5℃～25℃，第二剪切段的机筒温度在-5℃～35℃，第三物料输送段的机筒温度在0℃～45℃。
本发明合理设计软化剂的渗透和废胶粉的初步脱硫、脱硫工序和精炼工序三者，采用串联的螺杆挤出机作为废胶粉的脱硫再生生产设备，保证了废橡胶再生过程的安全连续化生产。软化剂与废胶粉初步混合后，在异向双螺杆中实现了软化剂的均匀渗透，由于缺少活化剂的作用分子链断裂较少，胶粉颗粒基本都处于均匀溶胀的初步脱硫状态，大分子链处于伸展状态；隔绝氧气加入第二台多螺杆挤出机中，在混合段利用活化剂与软化剂良好的相容性使活化剂均匀分散，在剪切段内温度下活化剂活性较大，通过活化剂和剪切作用实现脱硫再生，冷却后得到均匀脱硫的脱硫胶粉；胶粉经过脱硫后结构发生明显的变化，选择在第三台多螺杆挤出机中低温条件下进行精炼，避免了大分子主链的断裂的同时有效降低脱硫胶粉的门尼粘度，改善加工性能。
将软化剂和活化剂在不同位置依次加入，避免了以往同时加入活化剂和软化剂时，向废胶粉内部边渗透边反应引起的脱硫不均匀；软化剂均匀渗透得到的充分溶胀的胶粉颗粒分子链处于伸展状态，大幅降低了脱硫所需温度，在活化剂和剪切力的双重作用下选择性的打断S-S键，大大提高了脱硫效率的同时保证了力学性能；无核壳结构或硬质颗粒的脱硫胶粉能够快速降低门尼粘度，减少了精炼过程中能耗。
另外，异向双螺杆挤出机正位移输送能力强，可以合理调整渗透时间，具有的自清洁能力避免了长期使用后碳化结垢等引起的工艺变化，产品质量稳定，方便维护保养；在计算机模拟计算的基础上，通过螺纹元件的设计组合使物料在流向、流速上形成多重变化，设计了满足脱硫和精炼的两种要求的多螺杆挤出机，实现了密闭、连续和自动化。通过优化配方和工序，合理设计的装置克服了以往脱硫再生方法的缺陷，大幅降低能耗，整个制备流程在密闭隔氧条件下完成，所得再生胶性能优异，具有操作安全、简单、连续和节能、环保的优点。
附图说明
图1本发明系统示意图
1.保温输送计量装置；2.第一电机，3.第一减速机，4.异向双螺杆，5.异向双螺杆机筒，6.冷却输送装置，7.第二电机，8.第二减速机，9.多螺杆1，10.多螺杆机筒1，11.第三电机，12.第三减速机，13.多螺杆2，14.多螺杆机筒2，15.冷却输送装置，16.包装装置
图2异向双螺杆挤出机示意图
1.电机，2、联轴器，3.减速机，4.异向双螺杆，5.机筒，6.基座
图3同向平行三螺杆示意图
1.电机，2、联轴器，3.减速机，4.双螺杆，5.机筒，6.基座
图4同向双螺杆
1.电机，2、联轴器，3.减速机，4.螺杆，5.机筒，6.基座
具体实施方式
下面结合具体实施方式对本发明做进一步的描述。以下份数没有特别说明均为质量份数。
实施例：
采用废载重子午线轮胎胎面胶粉100份，加入煤焦油10份、松焦油10份为软化剂，于搅拌机内60℃下将胶粉与软化剂混合搅拌8min后，通过连续密闭保温输送计量装置将其加入第一台异向双螺杆挤出机，温度分别设定为加热排气段180℃、保温段为230℃、冷却段160℃，物料在挤出机内停留2min得到门尼粘度为195的初步脱硫胶粉，经冷却输送装置冷却至50℃，然后对接进入第二台同向双螺杆挤出机，从侧喂料加入0.1份活化剂2,2’-二硫化双(6-叔丁基对苯酚)，混合段的机筒温度在45℃，剪切段的机筒温度在70℃，冷却段的机筒温度在35℃，在挤出机内剪切的作用3min由机头挤出后得到门尼粘度110的脱硫胶粉，经过密闭连接冷却装置加入到第三台同向平行三螺杆挤出机，第一物料输送段的机筒温度为15℃，预剪切段的机筒温度为30℃，第二物料输送段的机筒温度为20℃，第二剪切段的机筒温度为25℃，第三物料输送段的机筒温度为15℃，芯轴温度为10℃，在挤出机内剪切的作用3min由机头挤出后，经成型装置和冷却装置使物料冷却至40℃，得到门尼粘度53的再生胶产品。
Figure BDA0001463652350000061
实施例2
采用废载重子午线轮胎胎面胶粉100份，加入妥尔油2份、松焦油3份为软化剂，于搅拌机内80℃下将胶粉与软化剂混合搅拌15min后，通过连续密闭保温输送计量装置将其加入第一台异向双螺杆挤出机，温度分别设定为加热排气段160℃、保温段为280℃、冷却段120℃，物料在挤出机内停留5min得到门尼粘度为180的初步脱硫胶粉，经冷却输送装置冷却至60℃，然后对接进入第二台同向双螺杆挤出机，从侧喂料加入3.0份活化剂二苯基二硫，混合段的机筒温度为55℃，剪切段的机筒温度为80℃，冷却段的机筒温度为40℃，在挤出机内剪切的作用3min由机头挤出后得到门尼粘度100的脱硫胶粉，经过密闭连接冷却装置加入到第三台同向平行三螺杆挤出机，第一物料输送段的机筒温度为15℃，预剪切段的机筒温度为30℃，第二物料输送段的机筒温度为20℃，第二剪切段的机筒温度为25℃，第三物料输送段的机筒温度为15℃，芯轴温度为10℃，在挤出机内剪切的作用3min由机头挤出后，得到门尼粘度62的再生橡胶产品。
Figure BDA0001463652350000062
实施例3：采用废载重子午线轮胎胎面胶粉100份，加入妥尔油8份、松焦油6份、松香4份为软化剂，于搅拌机内100℃下将胶粉与软化剂混合搅拌20min后，通过连续密闭保温输送计量装置将其加入第一台异向双螺杆挤出机，温度分别设定为加热排气段160℃、反应段为260℃、冷却段140℃，停留4min后物料挤出后得到门尼粘度为160的初步脱硫胶粉，经冷却输送装置冷却至55℃，然后对接进入第二台同向双螺杆挤出机，从侧喂料加入0.2份的活化剂正丁胺，混合段的机筒温度在65℃，剪切段的机筒温度在90℃，冷却段的机筒温度在50℃，在挤出机内剪切的作用3min由机头挤出后得到门尼粘度90的脱硫胶粉，然后对接进入第三台同向平行三螺杆挤出机，第一物料输送段的机筒温度为5℃，预剪切段的机筒温度为15℃，第二物料输送段的机筒温度为10℃，第二剪切段的机筒温度为20℃，第三物料输送段的机筒温度为15℃，芯轴温度为15℃，在挤出机内剪切的作用2min由机头挤出后，经成型装置和冷却装置使物料冷却至30℃，得到门尼粘度50的再生胶产品。
Figure BDA0001463652350000071

Claims (4)

1.一种多阶螺杆连续脱硫制备再生橡胶的方法，其特征在于，将废胶粉与软化剂于搅拌机内60℃～120℃下处理5min～25min后，进入60℃～120℃的保温缓冲罐内，经连续密闭保温输送计量装置进入到一台异向双螺杆挤出机内，在100℃～340℃停留1min～6min完成软化剂向胶粉内部的均匀渗透和废胶粉的初步脱硫，再经连续冷却装置在密闭条件下冷却至40℃～80℃，得到门尼粘度为100～230的初步脱硫物料，然后经连续输送至计量加料装置，进入第二台多螺杆挤出机内，通过侧喂料装置加入活化剂，控制多螺杆挤出机的机筒和芯轴的温度在20℃～110℃，1min～6min完成脱硫反应由挤出机挤出门尼粘度为70～150的脱硫胶粉，经连续冷却装置在密闭条件下冷却至25℃～60℃，进入第三台多螺杆挤出机内，控制多螺杆挤出机的机筒和芯轴的温度在-5℃～50℃，在剪切条件下精炼1～10min挤出后，再经成型装置和冷却装置使物料冷却至50℃以下后完成精炼工序，最终包装得到所需再生橡胶产品；
废胶粉与软化剂、活化剂的质量比为100:(2～20)：(0.01～3)；
软化剂是煤焦油、芳烃油、松焦油、妥尔油、环烷油、双戊烯、石蜡油、油酸、棉籽油、松香的一种或几者的混合物，活化剂是芳烃二硫化物、多烷基苯酚硫化物、苯基硫醇、胺基化合物的一种或几者的混合物；
所用的废胶粉是废载重子午线轮胎胶粉或废轿车胎胶粉的一种或二者的混合物；
异向双螺杆挤出机的加热排气段温度在120℃～200℃，保温段温度在200℃～340℃，冷却段温度在100℃～200℃。
2.根据权利要求1所述的方法，其特征是所述多螺杆挤出机是同向双螺杆挤出机或同向平行三螺杆挤出机中的一种。
3.根据权利要求1所述的方法，其特征是：第二台多螺杆挤出机混合段的机筒温度在40℃～70℃，剪切段的机筒温度在70℃～90℃，冷却段机筒温度在30℃～60℃。
4.根据权利要求1所述的方法，其特征是：第三台多螺杆挤出机第一物料输送段的机筒温度在0℃～25℃，预剪切段的机筒温度在5℃～40℃，第二物料输送段的机筒温度在5℃～25℃，第二剪切段的机筒温度在-5℃～35℃，第三物料输送段的机筒温度在0℃～45℃。
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