CN114367293A - 一种用于防老剂6ppd的椰壳炭载体贵金属催化剂 - Google Patents
一种用于防老剂6ppd的椰壳炭载体贵金属催化剂 Download PDFInfo
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Abstract
本发明属于精细化工技术领域,涉及一种应用在合成橡胶防老剂6PPD中以椰壳炭作为主要载体的贵金属催化剂。采用以椰壳炭作为主要载体的贵金属催化剂用于固定床装置合成防老剂6PPD,能够削减Al2O3载体带来的不利影响,也可以消除由于铜离子的流失对防老剂6PPD效果的影响。而且还能有效地抑制MIBK转化为MIBC的副反应,提高原料的利用率,合成条件更温和,与现有工艺对比,可真正做到节能降耗,提高产品质量。
Description
技术领域
本发明属于精细化工技术领域,涉及一种应用在合成橡胶防老剂6PPD中以椰壳炭作为载体的贵金属催化剂。
背景技术
防老剂6PPD作为高效多功能低毒产品主要应用于橡胶工业中,是目前橡胶防老剂中最重要的品种之一。它对臭氧和屈挠老化有很好的防护效能,对氧、热等一般老化和铜、锰等有害金属也有良好的防护作用。
目前的6PPD生产工艺中,多采用铜系催化剂生产,目前生产工艺中采用原料酮和4-氨基二苯胺在催化剂的作用下,在一定的还原体系下进行合成,催化剂的种类不同,生产的工艺条件、产品的质量和成本都有不同。要想在市场竞争中具有优势,提高产品质量和降低成本,对工艺和催化剂的选择就较为重要了。
因此,对合成对苯二胺类防老剂的催化剂选择就尤为重要了。对合成对苯二胺类防老剂的催化剂种类研究也越来越多,其中也提及了对于Al2O3、硅藻土等不同催化剂载体的应用。
CN102260176A介绍了一种使用Ni/Al2O3体系催化剂的防老剂6PPD连续化生产工艺,可用于防老剂6PPD的年产7500吨以上的生产。该工艺采用的是气液固三相固定床加氢反应器,反应温度165~230℃,压力为5.5~6.0MPa,物料酮胺比为2~4:1,氢油比为2000~5000:1。
US336684A和US4043942中也详细研究了Ni/硅藻土催化剂,发现RT培司与MIBK反应收率达75%,而添加某些酸如4-甲基苯磺酸和某些有机硫化合物如PhSMe后,防老剂6PPD的收率得到很大增加。
CN201010523996阐述了一种SiO2介孔中空纳米球载体在催化剂制备中的应用,其比表面积可达600~900m2/g、球体直径80~120nm,壁厚5~20nm,具有比表面积高、流动性良好的特点。
CN201310157602则探讨了一种以TiO2-SiO2为载体的锰基低温脱硝催化剂及其制备方法,其特点是SiO2的加入大大的增加了载体的比表面积,有利于活性物质在其表面的分散及稳定性,且以TiO2-SiO2为复合载体能提高催化剂的抗碱金属中毒性能。
目前,国内对苯二胺类防老剂的主要生产厂家:山东圣奥化工股份有限公司、中石化南京化学工业公司等主要生产厂家合成防老剂6PPD均主要采用Cu/Al2O3体系催化剂。
虽然Al2O3体系催化剂价格便宜且便于连续生产操作,但是生产过程中MIBK转化为MIBC的副反应较为剧烈,从而导致产品质量较差、收率较低、生产过程中会产生含醇的废液等。
发明内容
本发明的技术方案:一种应用在合成橡胶防老剂6PPD中以椰壳炭作为载体的贵金属催化剂。椰壳炭作为载体的贵金属催化剂合成防老剂6PPD,不但产品质量好,而且后续处理简单。由于化工行业环保的要求,开拓创新绿色清洁生产工艺具有一定的意义。
本发明方法的主要技术方案:用于防老剂6PPD的椰壳炭载体贵金属催化剂,其特征在于:所述的催化剂载体为椰壳炭,负载贵金属元素;椰壳炭为天然椰壳制成,含有Ca、Fe、S元素。
一般地,所述催化剂中贵金属含量0.1%~5%。
所述贵金属元素包括Pt、Pd。
所述椰壳炭比表面积≥1000m2/g,孔容0.3~2.5g/ml,孔径0.5~2.5nm,灰分≤5%,吸水率60%。
所述椰壳炭中Ca含量≤0.1%,Fe含量≤0.2%,S含量0.2~0.6%。
所述椰壳炭为粉末或成型。
本发明提供的催化剂用于合成防老剂6PPD。
所述反应原料为4-氨基二苯胺及与其相似的有机物,甲基异丁基甲酮、丙酮及其与其相似的有机物。
所述合成反应温度为80~200℃,压力为0.5~2.5MPa,优选0.8~2.0MPa。
所述物料酮胺摩尔比为1.5~5.5∶1,氢油比为2000~6000∶1。
本发明采用椰壳炭作为载体的贵金属催化剂合成防老剂6PPD,即将0.1%~5%铂系或钯系催化剂装入固定床反应装置中,以椰壳炭作为载体的贵金属催化剂合成防老剂6PPD和IPPD。
本发明采用椰壳炭作为载体的贵金属催化剂用于固定床装置或反应釜装置合成对苯二胺类防老剂,即能避免铜系催化剂带来的不利影响,还可以提高产品质量和节约原料,降低生产成本也可避免镍系催化剂原料利用率低,后续处理复杂等不利影响。椰壳炭作为载体的贵金属催化剂合成防老剂6PPD,提高了产品质量,有效的抑制副反应的,降低能耗,为防老剂6PPD的工业生产提供高效,节能、环保的新途径。
具体实施方式
下面结合实施例对本发明加以详细描述。
以下实施例中,采用椰壳炭作为载体的贵金属催化剂合成防老剂6PPD,椰壳炭为天然椰壳制成粉状,椰壳炭比表面积≥1000m2/g,孔容0.3~2.5g/ml,孔径0.5~2.5nm,灰分≤5%,吸水率60%。
将铂系催化剂装入固定床反应装置中,反应原料为4-氨基二苯胺及,甲基异丁基甲酮、丙酮,以椰壳炭作为载体的贵金属催化剂合成防老剂6PPD和IPPD。
实施例1
将含量为0.3%的Pt,Ca含量为0.05%,Fe含量为0.1%,S含量0.4%催化剂装入固定床反应装置中,加入相应的反应原料,反应温度为120℃,压力为2.0MPa,酮胺比为5.5∶1,氢油比为2000∶1进行对苯二胺类防老剂的合成试验,经色谱分析,反应转化率为99.99%,选择性为99.23%,酮醇比为99/1。
实施例2
将含量为0.4%的Pt,Ca含量为0.1%,Fe含量为0.2%,S含量0.6%催化剂装入固定床反应装置中,加入相应的反应原料,反应温度为120℃,压力为1.9MPa,酮胺比为4.5∶1,氢油比为2000∶1进行对苯二胺类防老剂的合成试验,经色谱分析,反应转化为99.51%,选择性均为98.86%,酮醇比为94/6。
实施例3
将含量为0.5%的Pt,Ca含量为0.05%,Fe含量为0.05%,S含量0.3%催化剂装入固定床反应装置中,加入相应的反应原料,反应温度为115℃,压力为1.8MPa,酮胺比为5.5∶1,氢油比为4000∶1进行对苯二胺类防老剂的合成试验,经色谱分析,反应转化为100%,选择性为98.75%,酮醇比为94/6,。
实施例4
将含量为1%的Pt,Ca含量为0.05%,Fe含量为0.05%,S含量0.2%催化剂装入固定床反应装置中,加入相应的反应原料,反应温度为115℃,压力为1.7MPa,酮胺比为5.5∶1,氢油比为3000∶1进行对苯二胺类防老剂的合成试验,经色谱分析,反应转化≥99.94%,选择性均≥98.21%,酮醇比为95/5。
实施例5
将含量为2%的Pt,Ca含量为0.1%,Fe含量为0.05%,S含量0.2%催化剂装入固定床反应装置中,加入相应的反应原料,反应温度为105℃,压力为1.5MPa,酮胺比为3.5∶1,氢油比为6000∶1进行对苯二胺类防老剂的合成试验,经色谱分析,反应转化率99.76%,选择性98.55%,酮醇比为93/7。
实施例6
将含量为3%的Pt,Ca含量为0.1%,Fe含量为0.2%,S含量0.6%催化剂装入固定床反应装置中,加入相应的反应原料,反应温度为105℃,压力为1.0MPa,酮胺比为5.5∶1,氢油比为5000∶1进行对苯二胺类防老剂的合成试验,经色谱分析,反应转化率99.69%,选择性98.91%,酮醇比为95/5,。
实施例7
将含量为5%的Pt,Ca含量为0.05%,Fe含量为0.1%,S含量0.5%催化剂装入固定床反应装置中,加入相应的反应原料,反应温度为110℃,压力为2.0MPa,酮胺比为2.5∶1,氢油比为3000∶1进行对苯二胺类防老剂的合成试验,经色谱分析,反应转化率99.59%,选择性98.31%,酮醇比为93/7。
实施例8
将含量为2%的Pt,Ca含量为0.05%,Fe含量为0.01%,S含量0.25%催化剂装入固定床反应装置中,加入相应的反应原料,反应温度为120℃,压力为1.5MPa,酮胺比为3.5∶1,氢油比为4000∶1进行对苯二胺类防老剂的合成试验,经色谱分析,反应转化率99.23%,选择性98.52%,酮醇比为93/7。
Claims (10)
1.一种用于防老剂6PPD的椰壳炭载体贵金属催化剂,其特征在于:所述的催化剂载体为椰壳炭,负载贵金属元素;椰壳炭为天然椰壳制成,含有Ca、Fe、S元素。
2.如权利要求1所述的催化剂,其特征在于:催化剂中贵金属含量0.1%~5%。
3.如权利要求1或2所述的催化剂,其特征在于:所述贵金属元素包括Pt、Pd。
4.如权利要求1所述的催化剂,其特征在于:椰壳炭比表面积≥1000m2/g,孔容0.3~2.5g/ml,孔径0.5~2.5nm,灰分≤5%,吸水率60%。
5.如权利要求1或4所述的催化剂,其特征在于:椰壳炭中Ca含量≤0.1%,Fe含量≤0.2%,S含量0.2~0.6%。
6.如权利要求1或4所述的催化剂,其特征在于:椰壳炭为粉末或成型。
7.如权利要求1所述催化剂的应用,其特征在于:用于合成防老剂6PPD。
8.如权利要求7所述的应用,其特征在于:反应原料为4-氨基二苯胺及与其相似的有机物,甲基异丁基甲酮、丙酮及其与其相似的有机物。
9.如权利要求7所述的应用,其特征在于:合成反应温度为80~200℃,压力为0.5~2.5MPa,优选0.8~2.0MPa。
10.如权利要求7所述的应用,其特征在于:物料酮胺摩尔比为1.5~5.5∶1,氢油比为2000~6000∶1。
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