CN108273567A - 轻质丙烯酸催化剂载体及其制备方法 - Google Patents
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Abstract
本发明公开了轻质丙烯酸催化剂载体,它由10‑20wt%的铝矾土、3‑5wt%的湖南浦口砂、3‑5wt%的半山泥、30‑40wt%的拟薄水铝石、10‑20wt%的江西东桥砂、10‑30wt%的高岭土、10‑20wt%的木粉,先将铝矾土、湖南浦口砂、半山泥和一半的高岭土经球磨混合,得到均匀的基料,再将上述基料搪制成坯体;再将拟薄水铝石粉、江西东桥砂、木粉和一半的高岭土经球磨混合得到均匀的面料,再将面料加入搪球机中继续搪制成球粒,在搪球机中加入非金属化合物晶体颗粒,再在球粒表面喷涂一层胶体后,将球粒高温烧制而成。它不仅吸水率大、比重小、比表面积大和吸附力强,且工艺简单,成本低。
Description
技术领域
本发明涉及石油化工及特种陶瓷行业,具体涉及一种轻质丙烯酸催化剂载体及其制备方法。
背景技术
丙烯酸是重要的有机合成原料及合成树脂单体,是聚合速度非常快的乙烯类单体。是最简单的不饱和羧酸,由一个乙烯基和一个羧基组成。纯的丙烯酸是无色澄清液体,带有特征的刺激性气味。它可与水、醇、醚和氯仿互溶,是由从炼油厂得到的丙烯制备的。大多数用以制造丙烯酸甲酯、乙酯、丁酯、羟乙酯等丙烯酸酯类。丙烯酸及丙烯酸酯可以均聚及共聚,其聚合物用于合成树脂、合成纤维、高吸水性树脂、建材、涂料等工业部门。
丙烯酸的工业生产方法由最早的氯乙醇法、氰乙醇法、高压Reppe法、改良Reppe法、烯酮法、丙烯腈水解法、乙烯法逐渐发展到当今的丙烯两步气相催化氧化法。目前,丙烯两步气相催化氧化法因具有技术先进、丙烯转化率高、丙烯酸收率高和能够长周期安全平稳运行等特点在工业生产中应用广泛。国内的工业丙烯酸生产方法均采用丙烯两步气相催化氧化法。丙烯两步气相催化氧化法是在复合金属氧化物催化剂存在下,丙烯经空气氧化生成丙烯醛,再进一步催化氧化成丙烯酸。催化剂是丙烯两步气相催化氧化法生产丙烯醛和丙烯酸的核心。
丙烯酸专用催化剂载体作为催化剂载体的一种,具有使制成的催化剂具有合适的形状、尺寸和机械强度,以符合工业反应器的操作要求,并且可使丙烯酸催化剂活性组分分散在载体表面上,获得较高的比表面积,提高单位质量活性组分的催化效率等优点。
当前丙烯酸催化剂载体主要依赖从日本等发达国家进口,导致市面上丙烯酸专用催化剂载体价格过高,并且由于进口的丙烯酸催化剂专用载体对载体的高抗压强度、轻堆积比重、高载体吸水率、大表观孔体积等物理性能指标要求,导致国内丙烯酸催化剂专用载体制备基本处于瓶颈阶段。
发明内容
本发明针对上述现有技术存在的问题,提供了一种气孔率高,密度低,强度高,比表面积大的轻质丙烯酸催化剂载体及其制备方法。
本发明要解决的技术问题采用的技术方案是 :轻质丙烯酸催化剂载体,它由以下原料组成:10-20wt%且粒度为100-150目的铝矾土、3-5wt%且粒度为50-100目的湖南浦口砂、3-5wt%的半山泥、30-40wt%且粒度为150-200目的拟薄水铝石、10-20wt%且粒度为150-200目的江西东桥砂、10-30wt%的高岭土、10-20wt%的木粉,按下述方法经混合,成型和烧结制备而成:
a、先将上述原料中的铝矾土、湖南浦口砂、半山泥和一半的高岭土经球磨混合,得到均匀的基料,
b、再将上述基料加入到搪球机中机械滚动制成4~4.5mm球料坯体;
c、再将上述原料中的拟薄水铝石粉、江西东桥砂、木粉和一半的高岭土经球磨混合,得到均匀的面料,
d、再将面料加入搪球机中将球料坯体继续搪制成8-12mm的球粒,
e、在搪球机中加入目数为50-100的非金属化合物晶体颗粒,在球粒表面喷涂一层胶体后,将球粒加入搪粒机中搪粒,使球粒形成一层粗糙的表面层,
f、将球粒放入烧结炉中,先将炉体温度先升到800℃,保温1-2小时,再升温至1100~1200℃,烧结1.5~2 小时,冷却后得到轻质丙烯酸催化剂载体。
本发明所述的高岭土的主要组成为 SiO2 45.76%~50.75%、Al2O3 36.65%~37.87%、Fe2O3 0.54%~1.59%、MgO 0.5%~0.67%、CaO 0.046%~0.2%、Na2O 1.22%~1.74%、K2O 1.56%~2.08%、TiO2 0.32%~1.09%等多种微量成分。
本发明所述的拟薄水铝石的主要成份Al2O3含量60-65%。
所述木粉为100-150目用木屑加工而成的粉料。
本发明所述湖南浦口砂为湖南省醴陵市浦口乡用当地的深层岩石经粉碎加工而成的粉末砂,其主要化学成份Al2O3大于14% ,Fe2O3不大于1.5%,钾钠含量不大于4.5%,其余为SiO2和其它杂质,体积密度1.5-2g/mm3。
本发明所述半山泥为江西省萍乡市南坑出产的矿瓷泥,青白色,有粘性,Al2O3大于16% ,Fe2O3不大于1.0%,钾钠含量不大于4.5%,SiO2大于72.79%和杂质,密度1.8-2.3g/cm3。
本发明所述江西东桥砂为江西省萍乡市东桥镇出产的一种用矿石经粉碎加工而成的粉末砂,粒度小于0.1毫米,主要化学成份Al2O3大于45% ,Fe2O3小于1.0%,余量为SiO2和其它杂质,密度大于2.55g/cm3。
所述非金属化合物晶体颗粒包括碳化硅、氮化硅、碳化钛。
本发明为球体或椭球体,其内层抗压强度高,质轻密度小,而外层比表积大,吸水性好,具有活性,采用二次加温煅烧工艺,使载体整体抗压强度高、组织细密不开裂。
本发明的机理原理:一是利用拟薄水铝石在400~700℃间分解的产品γ-Al2O3具有比表面高、孔容大等特点;于1100~1200℃间煅烧得到的纳米级α- Al2O3具有比表面低、粒度分布均匀、几乎没有催化活性,可以满足氧源和反应混合均匀分散的要求,利用拟薄水铝石的这种特性,加入熔剂含量较高的高岭土、以木粉为表面造孔剂,利用高岭土和膨润土的低温烧结特性制成烧结温度在850℃~1100℃的比表面积大、比重小、吸水率高、强度大的丙烯酸催化剂载体;二是在球体双层结构中分别加入一些特定性能的原料和使球体表面粘附有细小颗粒,从而大大提高球体表面的比表面积和吸附性,确保载体表面可充分吸附催化活性组份,制成比表面积大、比重小、吸水率高、强度大的丙烯酸催化剂载体。
本发明与现有技术相比具有的优点主要是:以这种方法所制得的丙烯酸催化剂载体相比于现有产品具有吸水率大、比重小、比表面积大和吸附力强的特点,不仅催化剂载体的表面更粗糙,而且吸附能力更强,比重更小。且有工艺简单,成本低廉的优点。
具体实施方式
下面对原料中的物质组分进行详明 :
高岭土
组分 | SiO2 | Al2O3 | Fe2O3 | MgO | CaO | Na2O | K2O | TiO2 | 烧失 |
含量 | 50.745 | 37.87 | 1.59 | 0.672 | 0.044 | 1.744 | 1.56 | 0.324 | 8.79 |
下面结合实施例对本发明做进一步详细的说明,
实施例 1 :
所述轻质丙烯酸催化剂载体,它由以下原料组成:15wt%且粒度为100-150目的铝矾土、4wt%且粒度为50-100目的湖南浦口砂、4wt%的半山泥、30wt%且粒度为150-200目的拟薄水铝石、14wt%且粒度为150-200目的江西东桥砂、20wt%的高岭土、13wt%的木粉,按下述方法经混合,成型和烧结制备而成:
a、先将上述原料中的铝矾土、湖南浦口砂、半山泥和一半的高岭土(即原料中的10wt%的高岭土)经球磨混合,得到均匀的基料,
b、再将上述基料加入到搪球机中机械滚动制成4~4.5mm球料坯体;
c、再将上述原料中的拟薄水铝石粉、江西东桥砂、木粉和一半的高岭土(即原料中的10wt%的高岭土)经球磨混合,得到均匀的面料,
d、再将面料加入搪球机中将球料坯体继续搪制成8-12mm的球粒,
e、在搪球机中加入目数为50-100的碳化钛晶体颗粒,再在球粒表面喷涂一层耐高温胶体后,将球粒加入搪粒机中搪粒,使球粒形成一层粗糙的表面层,
f、将球粒放入烧结炉中,先将炉体温度先升到800℃,保温1-2小时,再升温至1100~1200℃,烧结1.5~2 小时,冷却后得到轻质丙烯酸催化剂载体。
实施例1所制得载体经测试,轻质多孔陶瓷吸水率为103%,体积密度为1.36g/cm3,抗压强度为85N/颗,堆积密度0.77g/ml,比表面积 280 m2/g。
实施例2:
所述轻质丙烯酸催化剂载体,它由以下原料组成:10wt%且粒度为100-150目的铝矾土、3wt%且粒度为50-100目的湖南浦口砂、3wt%的半山泥、34wt%且粒度为150-200目的拟薄水铝石、10wt%且粒度为150-200目的江西东桥砂、25wt%的高岭土、15wt%的木粉,按下述方法经混合,成型和烧结制备而成:
a、先将上述原料中的铝矾土、湖南浦口砂、半山泥和一半的高岭土(即原料中的12.5wt%的高岭土)经球磨混合,得到均匀的基料,
b、再将上述基料加入到搪球机中机械滚动制成4~4.5mm球料坯体;
c、再将上述原料中的拟薄水铝石粉、江西东桥砂、木粉和一半的高岭土(即原料中的12.5wt%的高岭土)经球磨混合,得到均匀的面料,
d、再将面料加入搪球机中将球料坯体继续搪制成8-12mm的球粒,
e、在搪球机中加入目数为50-100的碳化硅晶体颗粒,再在球粒表面喷涂一层耐高温胶体后,将球粒加入搪粒机中搪粒,使球粒形成一层粗糙的表面层,
f、将球粒放入烧结炉中,先将炉体温度先升到800℃,保温1-2小时,再升温至1100~1200℃,烧结1.5~2 小时,冷却后得到轻质丙烯酸催化剂载体。
实施例2所制得载体经测试,轻质多孔陶瓷吸水率为82%,体积密度为1.56g/cm3,抗压强度为114N/颗,堆积密度0.82g/ml,比表面积 265 m2/g。
实施例3:
所述轻质丙烯酸催化剂载体,它由以下原料组成:18wt%且粒度为100-150目的铝矾土、3wt%且粒度为50-100目的湖南浦口砂、3wt%的半山泥、36wt%且粒度为150-200目的拟薄水铝石、16wt%且粒度为150-200目的江西东桥砂、10wt%的高岭土、15wt%的木粉,按下述方法经混合,成型和烧结制备而成:
a、先将上述原料中的铝矾土、湖南浦口砂、半山泥和一半的高岭土(即原料中的5wt%的高岭土)经球磨混合,得到均匀的基料,
b、再将上述基料加入到搪球机中机械滚动制成4~4.5mm球料坯体;
c、再将上述原料中的拟薄水铝石粉、江西东桥砂、木粉和一半的高岭土(即原料中的5wt%的高岭土)经球磨混合,得到均匀的面料,
d、再将面料加入搪球机中将球料坯体继续搪制成8-12mm的球粒,
e、在搪球机中加入目数为50-100的氮化硅晶体颗粒,再在球粒表面喷涂一层耐高温胶体后,将球粒加入搪粒机中搪粒,使球粒形成一层粗糙的表面层,
f、将球粒放入烧结炉中,先将炉体温度先升到800℃,保温1-2小时,再升温至1100~1200℃,烧结1.5~2 小时,冷却后得到轻质丙烯酸催化剂载体。
实施例3所制得载体经测试,轻质多孔陶瓷吸水率为91%,体积密度为1.43g/cm3,抗压强度为103N/颗,堆积密度0.69g/ml,比表面积 260 m2/g。
Claims (2)
1.轻质丙烯酸催化剂载体,它由以下原料组成:10-20wt%且粒度为100-150目的铝矾土、3-5wt%且粒度为50-100目的湖南浦口砂、3-5wt%的半山泥、30-40wt%且粒度为150-200目的拟薄水铝石、10-20wt%且粒度为150-200目的江西东桥砂、10-30wt%的高岭土、10-20wt%的木粉,按下述方法经混合,成型和烧结制备而成:
a、先将上述原料中的铝矾土、湖南浦口砂、半山泥和一半的高岭土经球磨混合,得到均匀的基料,
b、再将上述基料加入到搪球机中机械滚动制成4~4.5mm球料坯体;
c、再将上述原料中的拟薄水铝石粉、江西东桥砂、木粉和一半的高岭土经球磨混合,得到均匀的面料,
d、再将面料加入搪球机中将球料坯体继续搪制成8-12mm的球粒,
e、在搪球机中加入目数为50-100的非金属化合物晶体颗粒,再在球粒表面喷涂一层胶体后,将球粒加入搪粒机中搪粒,使球粒形成粗糙的表面层,
f、将球粒放入烧结炉中,先将炉体温度先升到800℃,保温1-2小时,再升温至1100~1200℃,烧结1.5~2 小时,冷却后得到轻质丙烯酸催化剂载体。
2.根据权利要求1所述的轻质丙烯酸催化剂载体,其特征是:所述非金属化合物晶体颗粒包括碳化硅、氮化硅、碳化钛。
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