CN106391139A - 一种电渗析法制备六羟基铂酸二(乙醇胺)水溶液的方法 - Google Patents
一种电渗析法制备六羟基铂酸二(乙醇胺)水溶液的方法 Download PDFInfo
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- 229940031098 ethanolamine Drugs 0.000 title abstract 3
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- LDMNYTKHBHFXNG-UHFFFAOYSA-H disodium;platinum(4+);hexahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Na+].[Na+].[Pt+4] LDMNYTKHBHFXNG-UHFFFAOYSA-H 0.000 abstract 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
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- B01J37/348—Electrochemical processes, e.g. electrochemical deposition or anodisation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
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Abstract
本发明公开了一种电渗析法制备六羟基铂酸二(乙醇胺)水溶液的方法,该方法在隔膜式电渗析槽中通过电渗析法制得稳定的六羟基铂酸钠或六羟基铂酸钾的水溶液,浓缩溶液,冷却析出黄色固体,抽滤,洗涤,干燥;将电渗析所得的固体完全水溶后,调pH至酸性,得到淡黄色沉淀,过滤,洗涤,真空干燥后得六羟基铂酸;将上述所得的六羟基铂酸溶于乙醇胺水溶液中,得黄色的六羟基铂酸二(乙醇胺)水溶液,产率大于96%;该方法所得产物的杂离子浓度小于100ppm;本发明具有能耗低、易批量放大、环境污染小、占地面积小以及产物水溶液稳定等优点,符合绿色化学的要求,而且在大规模工业生产中具有很大的应用价值。
Description
技术领域
本发明涉及一种贵金属铂催化剂的合成方法,特别涉及一种电渗析法制备六羟基铂酸二(乙醇胺)水溶液的方法。
背景技术
基于铂的贵金属催化剂广泛的应用于各个领域,如机动车尾气净化、石油化工、污水处理以及医药中间体等多个领域,尤其是尾气净化方面越来越受到学者们的广泛关注。目前,人们普遍认为在机动车排气管处安装尾气净化器是改善尾气污染的最佳方式之一。众所周知,净化器的核心材料是催化剂,其中贵金属铂催化剂被公认为是一种有效的活性材料成分。然而,铂催化剂价格昂贵且不易制备。因此,如何降低铂催化剂的用量、增加催化剂的活性以及提高催化剂的循环使用率是目前科研工作者们的重要研究课题。
大量研究表明,与含氯的铂催化剂相比,不含氯的铂催化剂具有显著的催化优势。当这两种催化剂老化后,含氯的催化剂的催化活性大大下降,同时氯会降低催化剂的耐高温性和使用寿命。其中,文献Applied Catalysis B: Environmental. 1996,10:53-68和Industrial & Engineering Chemistry Research. 2001,41:1967-1972以及张爱敏等人均对此做了相关报道。基于上述考虑,人们逐渐把目光投向不含氯的铂催化剂的合成。Pt(NO3)2作为无氯的铂催化剂被开发出来,然而,该催化剂不稳定,需现配现用,难以储存。此外,该催化剂制备过程需用大量的硝酸,易产生酸性气体,对载体材料有严重的腐蚀作用,从而影响催化性能,如文献Journal of Physical Chemstry B. 2003,107:1802-1813.中报道。目前,国际上普遍比较认可的一种不含氯的铂催化前驱体--六羟基铂酸二(乙醇胺)水溶液用于净化处理机动车尾气。该催化剂稳定性及水溶性好,不含对催化剂有害的杂质如氯和硝酸根等成分。因此,该催化前驱体具有良好的应用前景。
和传统制备方法相比,电渗析制备法具有显著的优势。该法操作简单,产率高、能耗低、环境污染小、占地面积小以及产物水质稳定等优点,较为符合绿色化学的要求,在大规模工业生产中具有很大的应用价值,同时,该法也是化工产品生产及纯化过程中的一个重要方法。化学浸渍法是工业制备该类催化剂的主要方法之一,一般来说,浸渍过程中存在强吸附时,前驱体会与载体之间形成物理键或化学键。这种强相互作用会使前驱体在负载材料上的分布接近原子分布,从而提高其分散度。该法操作简单、方便可行,是本发明的一个重要制备步骤之一。随着机动车辆的日益增多,六羟基铂酸二(乙醇胺)水溶液作为催化前驱体的需求也日益增加,因此,开发出一种产率高、成本低、污染小、能耗少、操作简单和易于分离的制备技术变得尤为重要。
发明内容
本发明的目的是发明一种电渗析制备六羟基铂酸二(乙醇胺)水溶液的方法,具体方案如下:
(1)采用电渗析法制备六羟基铂酸钠或六羟基铂酸钾
在隔膜式电渗析槽中,以镍或石墨作为阴极电极材料、钛或/和钌作为阳极电极材料。阴极液室内放置有浓度为1~5mol/L的氯铂酸、氯铂酸钠或氯铂酸钾溶液,阳极液室为一定浓度的NaOH或KOH溶液,其pH不小于8,隔膜为阳离子膜。经100~1000A/m2的电流密度、电压为5~15V以及电解温度为20~40℃的反应条件下电解,当阴极液室pH为8时,反应停止,制得六羟基铂酸钠或六羟基铂酸钾的水溶液;将该液浓缩后,置于冰箱,析出黄色固体,分别用纯净水和乙醇各洗涤三次,真空干燥后的粗品,产率为95.2~98.6%;
(2)称取步骤(1)制备的六羟基铂酸钠或六羟基铂酸钾,在搅拌条件下将其完全溶解于水中,接着用浓度为2mol/L硝酸或醋酸调pH至3.5~5.5,搅拌反应1h,得大量淡黄色沉淀,抽滤得淡黄色固体,分别用醋酸、纯净水以及丙酮各洗涤三次,真空干燥后得六羟基铂酸,产率为95.9~98.4%;
(3)将上述制得的六羟基铂酸加入到乙醇胺水溶液中,在搅拌条件下使其完全溶解,最终得到黄色透明溶液,其中乙醇胺和六羟基铂酸的摩尔比为2.00~2.15:1;该水溶液铂的含量为100~200mg/mL,产率大于96%。杂质钠的含量为83~97ppm,氯的含量为95~98ppm。
与现有技术相比,本发明的有益效果主要体现在:
本发明所述的电渗析法具有产率高、成本低、污染小、能耗少以及操作简单,且产物收率在95~97%之间,该方法所得产物的杂离子浓度小于100ppm;同时,该法合成的产品纯度高,工艺稳定,产品质量可靠,具有重要的经济和社会价值。
具体实施方式
下面结合具体实施例对本发明进行进一步描述,但本发明的保护范围并不仅限于此。
实施例1:制备六羟基铂酸二(乙醇胺)水溶液的方法
(1)在隔膜式电渗析槽中,以镍电极作为阴极、钛电极作阳极,其面积均为1dm2;阴极液室内放置有浓度1mol/L氯铂酸钠水溶液,阳极液室为pH为8的NaOH溶液,隔膜为Nafion902膜;经电流密度为1000A/m2、电压为15V以及电解温度为20℃的反应条件下电解,待阴极液室pH为8时,反应停止,得六羟基铂酸钠溶液粗品;将该液浓缩至原来体积的八分之一,置于冰箱,析出黄色固体,分别用冰的纯净水和乙醇各洗涤三次,真空干燥后的纯品,产率为95.2%;
(2)称取0.04mol 13.68g六羟基铂酸钠,在磁力搅拌条件下将其溶于25mL的纯净水,接着用浓度为2mol/L硝酸调pH至3.5,搅拌反应1h,得大量淡黄色沉淀;抽滤该淡黄色固体,分别用醋酸、纯净水以及丙酮各洗涤三次,真空干燥后得六羟基铂酸纯品,产率为95.9%;H8O6Pt的理论值为: H : 2.76,Pt: 56.85,实测值为:H: 2.88,Pt: 57.03,结果与理论值相符;
(3)配置体积分数为10%的乙醇胺水溶液100mL,其中乙醇胺的物质的量为1.63mol,称取六羟基铂酸2.39g(0.80mol),在搅拌条件下将其溶解在上述溶液,最终得到黄色透明溶液;经测试,铂的含量为124mg/mL,产率为96.1%,溶液pH为9.0,杂质钠的含量为92ppm,氯的含量为98ppm;将目标液密封在棕色瓶并于避光条件下储存。
实施例2:制备六羟基铂酸二(乙醇胺)水溶液的方法
(1)在隔膜式电渗析槽中,以石墨电极作为阴极、钌电极作阳极,其面积均为1dm2。阴极液室为浓度3.0mol/L氯铂酸钾水溶液,阳极液室是pH为9的KOH溶液,隔膜为Nafion117膜;经电流密度为500A/m2、电压为10V以及电解温度为30℃的反应条件下电解,当阴极液室pH为8时,反应停止,得六羟基铂酸钾水溶液;将该液浓缩至原来体积的八分之一,置于冰箱,析出黄色固体,分别用冰的纯净水和乙醇洗涤洗涤三次,真空干燥后的纯品,产率为97.6%;
(2)称取0.04mol 15.0g六羟基铂酸钠,在磁力搅拌条件下将其溶于25mL的纯净水,接着用浓度为2mol/L硝酸或醋酸调pH至4.5,搅拌反应1h,得大量淡黄色沉淀;抽滤得淡黄色固体,分别用醋酸、纯净水以及丙酮各洗涤三次,真空干燥后得六羟基铂酸纯品,产率为96.7%;H8O6Pt的理论值为: H:2.7,Pt:65.2,实测值为H: 2.6,Pt:65.3,结果与理论值相符;
(3)配置体积分数为14%的乙醇胺水溶液100mL,其中乙醇胺的物质的量为2.28mol,称取六羟基铂酸3.32g(1.11mol),在搅拌条件下将其溶解在上述溶液,最终得到黄色透明溶液。经测试,铂的含量为196mg/mL,产率为97.2%,溶液pH为10.0,杂质钾的含量为97ppm,氯的含量为94ppm;将目标液密封在棕色瓶并于避光条件下储存。
实施例3:制备六羟基铂酸二(乙醇胺)水溶液的方法
(1)在隔膜式电渗析槽中,以石墨电极作为阴极、钛钌电极作阳极,其面积均为1dm2。阴极液室为浓度5mol/L氯铂酸,阳极液室是pH为10的KOH溶液,隔膜为Nafion115膜。经300A/m2的电流密度、电压为6V以及电解温度为40℃的反应条件下电解,待阴极pH为8时,反应停止,得六羟基铂酸钾溶液粗品,将该液浓缩至原来体积的八分之一,置于冰箱,析出黄色固体,分别用纯净水和乙醇洗涤洗涤三次,真空干燥后的纯品,产率为98.6%;
(2)称取0.04mol 11.96g六羟基铂酸,在磁力搅拌条件下将其溶于25mL的纯净水,接着用浓度为2mol/L醋酸调pH至5.5,搅拌反应1h,得大量淡黄色沉淀;抽滤得淡黄色固体,分别用醋酸、纯净水以及丙酮各洗涤三次,真空干燥后得六羟基铂酸纯品,产率为98.4%。H8O6Pt的理论值为H:2.7,Pt:65.2,实测值为H :2.8,Pt:64. 9,结果与理论值相符;
(3)配置体积分数为8%的乙醇胺水溶液100mL,其中乙醇胺的物质的量为1.34mol,称取六羟基铂酸1.91g(0.64mol),在搅拌条件下将其溶解在上述溶液,最终得到黄色透明溶液;经测试,铂的含量为192mg/mL,产率为98.2%,溶液PH为8.5,杂质钾的含量为91ppm,氯的含量为89ppm。将目标液密封在棕色瓶并于避光条件下储存。
Claims (5)
1.一种电渗析法制备六羟基铂酸二(乙醇胺)水溶液的方法,其特征在于具体操作如下:
第一步,电渗析过程在由阴极液室和阳极液室组成的隔膜式电渗析槽中进行,其中,槽内阴电极提供氢氧根离子,与放置于阴极液室中的氯铂酸根原料反应得到六羟基铂酸盐,阳极液室中的阳极液为NaOH或KOH溶液,电解浴温为20~40℃,电流密度为100~1000A/m2,电压为5~15V,当阴极液室pH为8时,反应停止,制得六羟基铂酸钠或六羟基铂酸钾的水溶液,浓缩溶液,冷却析出黄色固体,洗涤干燥后得到六羟基铂酸钠或六羟基铂酸钾;
第二步,取六羟基铂酸钠或六羟基铂酸钾,在搅拌条件下完全溶解于水中,用酸调节pH至3.5~5.5,得淡黄色沉淀,过滤,洗涤,真空干燥后得六羟基铂酸;
第三步,取上述所得的六羟基氯铂酸,将其溶于乙醇胺水溶液,得到六羟基铂酸二(乙醇胺)水溶液,其中乙醇胺和六羟基铂酸的摩尔比为2.00~2.15:1。
2.根据权利要求1所述的电渗析法制备六羟基铂酸二(乙醇胺)水溶液的方法,其特征在于:NaOH或KOH溶液的pH不小于8。
3.根据权利要求1所述的电渗析法制备六羟基铂酸二(乙醇胺)水溶液的方法,其特征在于:氯铂酸根原料为浓度1~5mol/L的氯铂酸、氯铂酸钠或氯铂酸钾溶液。
4.根据权利要求1所述的电渗析法制备六羟基铂酸二(乙醇胺)水溶液的方法,其特征在于:阴极液室和阳极液室间的阳离子隔膜。
5.根据权利要求1所述的电渗析法制备六羟基铂酸二(乙醇胺)水溶液的方法,其特征在于:第二步中调节pH的酸为硝酸或醋酸,其浓度为2mol/L。
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