CN107486232A - 一种乙炔氢氯化的高分散度无汞催化剂及其制备方法 - Google Patents
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Abstract
本发明公开了一种乙炔氢氯化的高分散度无汞催化剂及其制备方法,该催化剂以AuCl3为主催化剂,纳米CeO2为分散剂、LaCl3为抗还原剂、InCl3为催化助剂、掺氮活性炭为载体,采用超声分散分步浸渍‑微波干燥的方法制备。该催化剂具有分散度高、抗积炭效果好、催化转化率高,使用寿命长、成本低的优点。
Description
技术领域
本发明涉及一种化工催化剂,特别是一种乙炔氢氯化的高分散度无汞催化剂及其制备方法。
背景技术
乙炔氢氯化法和乙烯氧氯化法是氯乙烯(VCM)生产过程中主要采用的合成方法,由于受我国“贫油、富煤、少气”资源结构的制约,目前约75%左右的氯乙烯(VCM)是采用乙炔氢氯化法制取的,但该路线一直主要以剧毒的氯化汞/活性炭为催化剂,存在严重的环境污染问题。2013年10月10日,在日本举行的由联合国环境规划署主办的《水俣公约》外交全权大会上,包括中国在内的92个国家和地区的代表签署《水俣公约》,携手控制和减少全球汞排放。因此,无汞催化剂的研发对于PVC行业的发展及汞减排都有重要意义。
现有乙炔氢氯化反应的无汞催化剂在使用过程中,在同等氯化金(AuCl3)含量的条件下,由于生产工艺、分散剂和载体等问题的影响,氯化金通常以团簇状的形式负载于载体表面,分散度偏低,导致成本偏高;在乙炔和氯化氢的混合气体与催化剂反应过程中,乙炔会与氯化金(AuCl3)发生还原反应,将氯化金(AuCl3)中的Au3+还原为Au0,从而导致催化剂失活;由于乙炔在反应过程中会发生自聚反应,造成自聚物沉积在催化活性点位上,导致催化剂失活;催化剂的催化转化率偏低。因此,现有的乙炔氢氯化法使用的催化剂存在分散度偏低、使用寿命较短、转化率不高以及催化剂使用成本偏高的缺点。
发明内容
本发明的目的在于,提供一种乙炔氢氯化的高分散度无汞催化剂及其制备方法。本发明的催化剂具有分散度较高、使用寿命长、转化率高以及降低催化剂使用成本的优点。
本发明的技术方案:一种乙炔氢氯化的高分散度无汞催化剂,所述催化剂采用主催化成分AuCl3、分散剂纳米CeO2、抗还原剂LaCl3、催化助剂InCl3和掺氮活性炭制成。
前述的一种乙炔氢氯化的高分散度无汞催化剂中,按重量份计算,采用AuCl30.05-0.2份、纳米CeO20.1-1份、LaCl30.12-0.5份、InCl30.1-0.5份和掺氮活性炭97.8-99.63份制成。
前述的一种乙炔氢氯化高分散度无汞催化剂,其特征在于:掺氮活性炭是由煤粉、石油焦、三聚氰胺按质量比为10:1:0.5-1经过搅拌、造粒、炭化、活化、漂洗和干燥制备的。
按照前述的一种乙炔氢氯化的高分散度无汞催化剂的制备方法,按以下步骤制备:
(a)将AuCl3、纳米CeO2、LaCl3和InCl3加入水中,混合均匀,得A品;
(b)使用A品对掺氮活性炭进行浸渍,得B品。
(c)对B品进行干燥,得乙炔氢氯化的高分散度无汞催化剂。
前述的制备方法中,所述步骤(b)中使用A品对掺氮活性炭进行浸渍,是将A品均分为2~3等分,在超声环境下分步对掺氮活性炭进行浸渍。
前述的制备方法中,所述步骤(c)中对B品进行干燥,是采用微波干燥,干燥至B品中水分含量小于0.3%。
与现有技术相比,①主催化剂AuCl3的纳米颗粒大小直接影响到乙炔氢氯化催化反应的转化率,通过加入纳米CeO2、采用超声分步浸渍以及采用微波干燥均有助于均控制AuCl3的粒径在0.3nm左右,可提高分散度;
②造成氯化金催化剂失活的主要原因之一为乙炔自聚造成的积炭,自聚物沉积在活性点位上,阻挡了乙炔和氯化氢混合气体与氯化金活性点位的接触,通过添加纳米CeO2有助于抗积炭现象的发生,可延长催化剂的使用寿命;
③乙炔气体与氯化氢气体在AuCl3催化剂接触过程中,乙炔易将AuCl3中的Au3+还原为Au0从而导致失去活性,LaCl3为抗还原剂,可以增强对HCl的吸附能力,抑制AuCl3中的Au3+向Au0的转变,从而保持催化剂中有效成分的活性,可提高催化剂的转化率,并且延长了催化剂的使用寿命,降低了催化剂的使用成本;
④通过将InCl3作为催化助剂加入,可以增加AuCl3电子云的密度,形成双核桥式络合物,可提高催化剂的催化转化率;
⑤通过选用掺氮活性炭作为载体,掺氮活性炭中的氮原子作为供电子体影响着周围碳原子和负载的催化活性组分的同时,对活性组分具有锚定作用。
综上所述,本发明的催化剂具有分散度较高、使用寿命长、转化率高以及降低催化剂使用成本的优点。
具体实施方式
以下将对本发明的优选实施例进行详细的描述。应当理解,优选实施例仅为了说明本发明,而不是为了限制本发明的保护范围。
实施例1。乙炔氢氯化的高分散度无汞催化剂,按重量份计算,采用AuCl30.05份、纳米CeO20.14份、LaCl30.12份、InCl30.11份和掺氮活性炭99.58份制成。
所述的掺氮活性炭是由煤粉、石油焦、三聚氰胺按质量比为10:1: 0.5经过搅拌、造粒、炭化、活化、漂洗和干燥制备的。
乙炔氢氯化的高分散度无汞催化剂的制备方法,按以下步骤制备:
(a)将上述重量份的AuCl3、纳米CeO2、LaCl3和InCl3加入水中,混合均匀,得A品;
(b)将A品均分为2等分,在超声环境下分步对掺氮活性炭进行浸渍,的B品。
(c)采用微波干燥的方式对B品进行干燥,干燥至B品中水分含量为0.27%,得乙炔氢氯化的高分散度无汞催化剂。
以此重量份的原料制得的乙炔氢氯化的高分散度无汞催化剂,用于乙炔与氯化氢的加成反应时,在乙炔空间流速为20h-1,乙炔与氯化氢分子比为1:1.15的条件下,测定其催化转化率为98%。
实施例2。乙炔氢氯化的高分散度无汞催化剂,按重量份计算,采用AuCl30.1份、纳米CeO20.28份、LaCl30.24份、InCl30.22份和掺氮活性炭99.16份制成。
所述的掺氮活性炭是由煤粉、石油焦、三聚氰胺按质量比为10:1: 0.8经过搅拌、造粒、炭化、活化、漂洗和干燥制备的。
乙炔氢氯化的高分散度无汞催化剂的制备方法,按以下步骤制备:
(a)将上述重量份的AuCl3、纳米CeO2、LaCl3和InCl3加入水中,混合均匀,得A品;
(b)将A品均分为2等分,在超声环境下分步对掺氮活性炭进行浸渍,的B品。
(c)采用微波干燥的方式对B品进行干燥,干燥至B品中水分含量为0.24%,得乙炔氢氯化的高分散度无汞催化剂。
以此重量份的原料制得的乙炔氢氯化的高分散度无汞催化剂,用于乙炔与氯化氢的加成反应时,在乙炔空间流速为20h-1,乙炔与氯化氢分子比为1:1.15的条件下,测定其催化转化率为98.5%。
实施例3。乙炔氢氯化的高分散度无汞催化剂,按重量份计算,采用AuCl30.15份、纳米CeO20.42份、LaCl30.36份、InCl30.33份和掺氮活性炭98.74份制成。
所述的掺氮活性炭是由煤粉、石油焦、三聚氰胺按质量比为10:1: 1经过搅拌、造粒、炭化、活化、漂洗和干燥制备的。
乙炔氢氯化的高分散度无汞催化剂的制备方法,按以下步骤制备:
(a)将上述重量份的AuCl3、纳米CeO2、LaCl3和InCl3加入水中,混合均匀,得A品;
(b)将A品均分为3等分,在超声环境下分步对掺氮活性炭进行浸渍,的B品。
(c)采用微波干燥的方式对B品进行干燥,干燥至B品中水分含量为0.28%,得乙炔氢氯化的高分散度无汞催化剂。
以此重量份的原料制得的乙炔氢氯化的高分散度无汞催化剂,用于乙炔与氯化氢的加成反应时,在乙炔空间流速为20h-1,乙炔与氯化氢分子比为1:1.15的条件下,测定其催化转化率为99%。
Claims (7)
1.一种乙炔氢氯化的高分散度无汞催化剂,其特征在于:所述催化剂由主催化成分AuCl3、分散剂纳米CeO2、抗还原剂LaCl3、催化助剂InCl3和掺氮活性炭载体制成。
2.根据权利要求1所述的一种乙炔氢氯化的高分散度无汞催化剂,其特征在于:按重量份计算,采用AuCl30.05-0.2份、纳米CeO20.1-1份、LaCl30.12-0.5份、InCl30.1-0.5份和掺氮活性炭97.8-99.63份制成。
3.根据权利要求1或2所述的一种乙炔氢氯化高分散度无汞催化剂,其特征在于:掺氮活性炭是由煤粉、石油焦、三聚氰胺按质量比为10:1:0.5-1经过搅拌、造粒、炭化、活化、漂洗和干燥制备的。
4.根据权利要求1所述的一种乙炔氢氯化的高分散度无汞催化
剂及其制备方法,其特征在于:AuCl3、纳米CeO2、LaCl3和InCl3的物质的量比为:1:5:3:3。
5.按照权利要求1至3任一权利要求所述的一种乙炔氢氯化的高分散度无汞催化剂的制备方法,其特征在于:按以下步骤制备:
(a)将AuCl3、纳米CeO2、LaCl3和InCl3加入水中,混合均匀,得A品;
(b)使用A品对掺氮活性炭进行浸渍,得B品;
(c)对B品进行干燥,得催化剂。
6.根据权利要求4所述的制备方法,其特征在于:所述步骤(b)中使用A品对掺氮活性炭进行浸渍,是将A品均分为2~3等分,在超声环境下分步对掺氮活性炭进行浸渍。
7.根据权利要求4所述的制备方法,其特征在于:所述步骤(c)中对B品进行干燥,是采用微波干燥,干燥至B品中水分含量小于0.3%。
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