CN100469771C - 橡胶硫化促进剂mbt的精制方法 - Google Patents

橡胶硫化促进剂mbt的精制方法 Download PDF

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CN100469771C
CN100469771C CNB200710057731XA CN200710057731A CN100469771C CN 100469771 C CN100469771 C CN 100469771C CN B200710057731X A CNB200710057731X A CN B200710057731XA CN 200710057731 A CN200710057731 A CN 200710057731A CN 100469771 C CN100469771 C CN 100469771C
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CN101108834A (zh
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王树华
王树领
王树恒
孟庆保
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Kemai Chemical Co Ltd
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TIANJIN KEMAI CHEMICAL CO Ltd
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Abstract

本发明公开了一种橡胶硫化促进剂MBT的精制方法。该方法过程包括：按粗MBT与乙醇的质量比为1∶2～4，将质量含量为50～80%的粗MBT在20～70℃、转速为200～1200转/分钟的条件下，溶解于乙醇中，待完全溶解后，将溶液降温至10～50℃；将降温后的溶液加入到10～100℃的去离子水中，搅拌致使MBT发生沉淀，静置2～24小时，过滤、水洗、在20～100℃下干燥后得到精制的硫化促进剂MBT。本发明的优点在于：该方法过程简单，易于工业化，所制得的精制MBT纯度达到99.5%以上、熔点高、熔程短。

Description

橡胶硫化促进剂MBT的精制方法
技术领域
本发明涉及一种橡胶硫化促进剂2-硫醇基苯并噻唑(MBT)的精制方法，属于橡胶硫化促进剂MBT精制技术领域。
背景技术
随着橡胶工业的发展，硫化促进剂的研究与生产越来越受到人们的重视。硫化促进剂在橡胶硫化过程中起着非常重要的作用，它能大大加快橡胶与硫化剂的反应，提高生产率，同时也能改善硫化橡胶的物理机械性能，MBT是目前橡胶工业必不可少的一种主要促进剂。通常情况下，该促进剂中的杂质主要为树脂和中间产物(如苯并噻唑)，杂质的存在使得产品质量不高。文献(精细化工原料及中间体，2003，1:40)报道了精制MBT的方法。将粗MBT熔化物溶解在甲苯和氢氧化钠水溶液的混合物中，相分离，用甲苯萃取水相；用硫酸将MBT从MBT钠盐溶液中沉淀出来，即可得到精制的MBT。此方法只能除去少量的树脂及杂质，精制后的MBT纯度不高。文献(橡胶助剂，2003，2：21)报道了从废水中提纯MBT的方法。将粗MBT用氢氧化钠溶液溶解，静置后过滤，以达到除去树脂的目的，向滤液中加入稀硫酸使MBT析出，过滤、水洗至中性后得到精制的MBT。精制出杂质含量低、熔点高、熔程短的MBT是实现精制MBT广泛应用的关键。
发明内容
本发明的目的在于提供一种橡胶硫化促进剂MBT的精制方法，该方法操作简单，制得的MBT纯度高、熔点高、熔程短。
为达到上述目的，本发明通过下述技术方案加以实现：一种橡胶硫化促进剂MBT的精制方法，其特征在于包括以下过程：
1.按粗MBT与乙醇的质量比为1：2～4，将质量含量为50～80％的粗MBT在20～70℃、转速为200～1200转/分钟的条件下，溶解于乙醇中，待完全溶解后，将溶液降温至10～50℃；
2.将降温后的溶液加入到10～100℃的去离子水中，搅拌致使MBT发生沉淀，静置2～24小时，过滤、水洗、在20～100℃下干燥后得到精制的硫化促进剂MBT。
本发明的优点在于：该方法过程简单，易于工业化，所制得的精制MBT纯度达到99.5％以上、熔点高、熔程短。
具体实施方式
例1：
用苯胺与二硫化碳、硫磺在270～280℃，压力9～10Mpa条件下进行缩合反应，生成质量含量为75％的粗MBT，其余杂质包括：树脂20％、中间产物5％。将15克质量含量为75％的粗MBT，在30℃、转速为300转/分钟的条件下，溶解于200ml乙醇中，搅拌20分钟使MBT完全溶解。将溶液降温至10℃后，倒入200ml、10℃的去离子水中，用玻璃棒搅拌均匀，这时MBT沉淀出来，静置12小时。过滤、水洗，得到滤饼，滤饼在90℃下干燥后得到13.9克的硫化促进剂MBT。该2-硫醇基苯并噻唑促进剂的质量含量为99.6％、熔点为182.3℃。
例2：
本实施例所采用的粗MBT与实施例1相同，将15克质量含量为75％的粗MBT，在30℃、转速为300转/分钟的条件下，溶解于200ml乙醇中，搅拌20分钟使MBT完全溶解。将溶液降温至10℃后，倒入400ml、10℃的去离子水中，用玻璃棒搅拌均匀，这时MBT沉淀出来，静置24小时。过滤、水洗，得到滤饼，滤饼在90℃下干燥后得到14.1克的硫化促进剂MBT。该2-硫醇基苯并噻唑促进剂的质量含量为99.2％、熔点为181.5℃。
例3：
本实施例所采用的合成粗MBT的工艺与实施例1相同。将10克纯度为80％的粗MBT在60℃、转速为800转/分钟的条件下，溶解于800ml乙醇中，搅拌10分钟使MBT完全溶解。将溶液降温至20℃后，倒入800ml、40℃的去离子水中，用玻璃棒搅拌均匀，这时MBT沉淀出来，静置16小时。过滤、水洗，得到滤饼，滤饼在70℃下干燥后得到8.6克精制的硫化促进剂MBT。该2-硫醇基苯并噻唑促进剂的质量含量为98.9％、熔点为180.2℃。
例4：
本实施例所采用的粗MBT与实施例3相同，将10克纯度为80％的粗MBT在60℃、转速为800转/分钟的条件下，溶解于800ml乙醇中，搅拌10分钟使MBT完全溶解。将溶液降温至20℃后，倒入200ml、20℃的去离子水中，用玻璃棒搅拌均匀，这时MBT沉淀出来，静置8小时。过滤、水洗，得到滤饼，滤饼在90℃下干燥后得到9.1克精制的硫化促进剂MBT。该2-硫醇基苯并噻唑促进剂的质量含量为99.1％、熔点为181.1℃。

Claims (2)

1.一种橡胶硫化促进剂MBT的精制方法，其特征在于包括以下过程：
1).按粗MBT与乙醇的质量比为1：2～4，将质量含量为50～80％的粗MBT在20～70℃、转速为200～1200转/分钟的条件下，溶解于乙醇中，待完全溶解后，将溶液降温至10～50℃；
2).将降温后的溶液加入到10～100℃的去离子水中，搅拌致使MBT发生沉淀，静置2～24小时，过滤、水洗、在20～100℃下干燥后得到精制的硫化促进剂MBT，上述质量含量为50～80％的粗MBT是用苯胺与二硫化碳、硫磺在270～280℃，压力9～10Mpa条件下进行缩合反应得到的。
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CN101307037B (zh) * 2008-06-13 2010-08-18 天津大学 橡胶硫化促进剂m生产过程中的脱水方法
CN101759661B (zh) * 2009-11-16 2012-08-15 天津市科迈化工有限公司 熔融结晶提纯橡胶硫化促进剂mbt的方法
CN102675242A (zh) * 2012-05-08 2012-09-19 中国石油化工股份有限公司 一种硫化促进剂m的精制方法
CN102718728B (zh) * 2012-07-01 2015-06-17 山东尚舜化工有限公司 橡胶硫化促进剂mbt的精制工艺
CN102827103A (zh) * 2012-09-25 2012-12-19 科迈化工股份有限公司 医药中间体mbt的生产方法
CN104086506A (zh) * 2014-07-03 2014-10-08 江西凯利化工有限公司 一种非水极性法促进剂m的生产工艺
CN104211658B (zh) * 2014-09-15 2019-05-10 河南省开仑化工有限责任公司 新型橡胶硫磺促进剂mbt的制作方法
CN105061357A (zh) * 2015-08-05 2015-11-18 青岛科技大学 一种2-巯基苯并噻唑的精制方法
CN110845441A (zh) * 2019-11-12 2020-02-28 内蒙古科迈化工有限公司 一种双氧水法精制橡胶促进剂mbt的方法
CN110698428A (zh) * 2019-11-12 2020-01-17 内蒙古科迈化工有限公司 一种制备橡胶促进剂mbts的方法
CN115403827A (zh) * 2022-08-02 2022-11-29 山东戴瑞克新材料有限公司 一种m树脂的处理方法

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