CN105289750A - 一种油溶性加氢催化剂及其制备方法和用途 - Google Patents
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Abstract
本发明涉及一种油溶性加氢催化剂及其制备方法和用途,所述催化剂包括以下成分:VIII族和VIB族金属化合物中的一种或几种、羧酸类有机物和醇类有机物中的一种或几种、和硫化剂,其中金属元素的质量在催化剂中的重量含量为0.5-15%,所述硫化剂为液硫或能在硫化条件下分解成H2S的不稳定硫化物,硫化剂中元素硫的质量为催化剂中金属元素质量的0.8-4倍。本发明的催化剂成本低,制备简单,分散性能好,与原料接触面积大,推广前景良好。
Description
技术领域
本发明涉及一种加氢催化剂,属于石油化工和煤化工领域。
背景技术
近年来浆态床加氢技术成为研究热点,该技术可应用于重油加氢、油煤混炼和煤直接液化工艺中,在该工艺中催化剂是核心技术之一,因此有必要对其进行深入研究。由于浆态床加氢工艺特点:原料(尤其是油煤混炼和煤直接液化工艺)的黏度高、流动性差,催化剂的分散性成为发挥其活性的关键因素之一,由于油溶性催化剂能够与反应原料混溶,其分散性能够得到最大程度的发挥,但油溶性催化剂较高的合成成本是制约其快速发展的重要因素。
发明内容
为了解决上述问题,本发明提供一种油溶性加氢催化剂及其制备方法和用途,能够大幅的降低成本。
本发明的技术方案如下:
一种油溶性加氢催化剂,其特征在于包括以下成分:VIII族和VIB族金属化合物中的一种或几种、羧酸类有机物和醇类有机物中的一种或几种、和硫化剂,其中金属元素的质量在催化剂中的重量含量为0.5-15%,所述硫化剂为液硫或能在硫化条件下分解成H2S的不稳定硫化物,硫化剂中元素硫的质量为催化剂中金属元素质量的0.8-4倍。
所述金属优选为:Fe、Co、Ni、Ru、Pd、Pt、Cr、Mo、W中的一种或几种。
所述金属进一步优选为钼和铁。
所述有机物优选为:C2-C6的羧酸,C2-C5的单醇、二醇、三醇中的一种或几种。
所述硫化剂优选为C2S或二甲基二硫醚。
当所述催化剂使用于重油加氢时,还包括吸附剂,所述吸附剂为具有吸附能力的粉末状物质催化剂,吸附剂添加量为反应物的1%-10%。
上述吸附剂优选为碳纤维、煤粉、活性碳粉、炭黑粉中的一种或几种的混合物。
上述的一种油溶性加氢催化剂的制备方法,其特征在于包括以下步骤:
(1)将无机金属盐配制成水溶液;
(2)调整溶液PH值为碱性;
(3)将溶液干燥,去除水分,并研磨成300μm以下的粉末;
(4)将干燥后的金属盐与有机物在230-260℃下搅拌≥1.2小时。
优选的所述无机金属盐为钼酸铵和硝酸铁,金属Mo与Fe的质量比为1:1.5~2.5;通过向溶液中添加氨水,使溶液PH=8~9。
上述催化剂的用途,其特征在于用于煤直接液化工艺、油煤混炼工艺和重油加氢工艺,煤直接液化工艺指以煤为原料,以煤液化的循环油为供氢溶剂进行加工;油煤混炼工艺指以原油、常压渣油、减压渣油、催化油浆、脱油沥青和煤焦油中的一种或者多种组合与褐煤、烟煤中的一种或者多种组合为原料进行加工,油与煤的比例范围为97-30:3-70;重油加氢工艺指以原油、常压渣油、减压渣油、催化油浆、脱油沥青和煤焦油中的一种或者多种组合为原料进行加工。
本发明的一种油溶性有机金属催化剂,包括:VIII族和VIB族金属催化剂、硫化剂和适当有机物,对于重油浆态床加氢,由于结焦物可能堵塞管道和设备,并对设备、泵和阀造成严重地磨损,需要酌情添加吸附剂以吸附结焦物,并带离系统。对于油煤混炼和煤直接液化工艺,由于作为反应物的煤粉自身可作为吸附剂,所以不需要额外添加吸附剂。吸附剂需要能参与反应的物质,优先选择碳纤维、煤粉、活性碳粉、炭黑粉、焦炭粉,并且这些物质的密度和硬度都比较小,不会对设备造成严重的磨损。硫化剂可在任何方便的时刻加入,例如在催化剂制备过程中与其他成分混合,也可以与上述制备步骤完成后的产物共同添加到加氢反应物中。
本发明的催化剂采用VIII族和VIB族金属作为催化剂主要成分,其均能起到催化效果,根据成本和催化效率优选为铁和钼,在本发明所选取的特定的有机物和硫化剂作用下,其分散性能好,与原料接触面积大,原料煤和/或油的加氢裂化程度较深,同时还大大降低了原料和催化剂对设备、泵、阀和管道的磨损,从数次中试试验结果来看,本发明提供的催化剂是实用和可靠的。同时,本发明的催化剂成本低,制备简单,推广前景良好。
具体实施方式
为进一步阐述本发明的具体特征,下面将结合具体实例来写详细叙述。
实施例1
一种油溶性Mo-Fe双金属催化剂,该催化剂是由钼酸铵和硝酸铁组成的油溶性金属催化剂,Mo与Fe质量比为1:2,金属在催化剂中的重量含量为4.5%,制备方法包括以下步骤:
1、将钼酸铵和硝酸铁配制成水溶液,保证金属Mo与Fe的质量比为1:2;
2、向溶液中注入氨水,使PH=8.8;
3、将溶液在110℃下真空干燥,去除水分,并研磨成300μm以下的粉末;
4、将干燥后的金属盐与1,3-丙二醇在230-260℃下搅拌,边搅拌变反应,反应时间≥1.2小时。
通过本方法制得的催化剂Mo质量分数为1.5%,Fe的质量分数为3.0%。
将制得的催化剂用到油煤混炼工艺中,油为减压渣油,其性质见表1,煤为烟煤,其性质见表2,催化剂添加量(元素Mo与Fe的总质量与反应物的质量比)为0.8‰,硫化剂添加量为1.6‰,不添加吸附剂。
表1.减压渣油的基本性质表
表2.煤的基本性质表
3、反应结果数据表:
气产率,wt% | 5.53 |
萃取油收率,wt% | 89.15 |
油煤焦产率,wt% | 5.32 |
装置连续运转8000小时,设备、泵、阀和管道无堵塞和明显的磨损现象。
实施例2
本实施例为如实施例1所述减压渣油加氢,采用如实施例1制备的催化剂再添加5%活性碳粉作为吸附剂,反应结果及装置磨损情况均基本与实施例1相同。
结论:
从上述实施例可以看出,本发明的金属有机催化剂制备方法简单,原料成本低,添加量少,实验过程中原料和催化剂对设备、泵、阀和管道的磨损较低,萃取油收率均可达到89%以上,残渣仅为5%左右,该催化剂值得大力推广。
以上所述仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,可轻易想到的变化或替换,例如金属和类似性质的有机物的替换以及各成分不同的配比等都应涵盖在本发明的保护范围之内。因此,本发明的保护范围应该以权利要求书的保护范围为准。
Claims (10)
1.一种油溶性加氢催化剂,其特征在于包括以下成分:VIII族和VIB族金属化合物中的一种或几种、羧酸类有机物和醇类有机物中的一种或几种、和硫化剂,其中金属元素的质量在催化剂中的重量含量为0.5-15%,所述硫化剂为液硫或能在硫化条件下分解成H2S的不稳定硫化物,硫化剂中元素硫的质量为催化剂中金属元素质量的0.8-4倍。
2.根据权利要求1所述的催化剂,其特征在于所述金属为:Fe、Co、Ni、Ru、Pd、Pt、Cr、Mo、W中的一种或几种。
3.根据权利要求2所述的催化剂,其特征在于所述金属为钼和铁。
4.根据权利要求1所述的催化剂,其特征在于所述有机物为:C2-C6的羧酸,C2-C5的单醇、二醇、三醇中的一种或几种。
5.根据权利要求1所述的催化剂,其特征在于所述硫化剂为C2S或二甲基二硫醚。
6.根据权利要求1所述的催化剂,其特征在于所述催化剂使用于重油加氢,还包括吸附剂,所述吸附剂为具有吸附能力的粉末状物质催化剂,吸附剂添加量为反应物的1%-10%。
7.根据权利要求6所述的催化剂,所述吸附剂为碳纤维、煤粉、活性碳粉、炭黑粉中的一种或几种的混合物。
8.根据权利要求1-7任一所述的一种油溶性加氢催化剂的制备方法,其特征在于包括以下步骤:
(1)将无机金属盐配制成水溶液;
(2)调整溶液PH值为碱性;
(3)将溶液干燥,去除水分,并研磨成300μm以下的粉末;
(4)将干燥后的金属盐与有机物在230-260℃下搅拌≥1.2小时。
9.根据权利要求8所述的催化剂,其特征在于所述无机金属盐为钼酸铵和硝酸铁,金属Mo与Fe的质量比为1:1.5~2.5;通过向溶液中添加氨水,使溶液PH=8~9。
10.根据权利要求1-7任一所述的催化剂的用途,其特征在于用于煤直接液化工艺、油煤混炼工艺和重油加氢工艺,煤直接液化工艺指以煤为原料,以煤液化的循环油为供氢溶剂进行加工;油煤混炼工艺指以原油、常压渣油、减压渣油、催化油浆、脱油沥青和煤焦油中的一种或者多种组合与褐煤、烟煤中的一种或者多种组合为原料进行加工,油与煤的比例范围为97-30:3-70;重油加氢工艺指以原油、常压渣油、减压渣油、催化油浆、脱油沥青和煤焦油中的一种或者多种组合为原料进行加工。
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CN110237850A (zh) * | 2018-03-07 | 2019-09-17 | 中国石油天然气股份有限公司 | 一种加氢裂化催化剂的制备方法 |
CN110237862A (zh) * | 2018-03-07 | 2019-09-17 | 中国石油天然气股份有限公司 | 一种制备加氢裂化催化剂的方法 |
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CN103372455A (zh) * | 2012-04-26 | 2013-10-30 | 中国石油化工股份有限公司 | 一种加氢催化剂及其制备和应用 |
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CN107033955A (zh) * | 2017-05-27 | 2017-08-11 | 北京中科诚毅科技发展有限公司 | 一种采用全能床加氢工艺的全厂工艺流程 |
CN109207183A (zh) * | 2017-06-30 | 2019-01-15 | 昆山超优清洁能源有限公司 | 一种复合型油溶性催化剂在油煤共炼工艺中的使用方法 |
CN110237850A (zh) * | 2018-03-07 | 2019-09-17 | 中国石油天然气股份有限公司 | 一种加氢裂化催化剂的制备方法 |
CN110237862A (zh) * | 2018-03-07 | 2019-09-17 | 中国石油天然气股份有限公司 | 一种制备加氢裂化催化剂的方法 |
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